實驗記錄英文寫作模板

1、Sentence Template for Notebook and Report WritingPfizer Project Management TeamApril 12,2007Part 1:反應(yīng)前的裝置描述1.1: A 3 L three-necked round bottom flask equipped with mechanical stirrer (or magneticstirrer), addition funnel and thermometer (or DeanStock; drying tube)1.2: All flasks used in the reaction

2、 were heated under vacuum for 30 minutes and purged withN2for 10 minutes.(無水反應(yīng)裝置)Part 2:加料2.1:不同的順序和表達(dá)2.1.1: A 3 L three-necked round bottom flask equipped with mechanical stirrer (or magneticstirrer), addition funnel and thermometer (or Dean-Stock; drying tube) were charged with A(10 mL, 1 mole), B

3、 (2 g, mole) and C (50 mL),2.1.1.1: a solution of D (10 g, I mole) in E (20 mL) was added dropwise (via addition funnelor syringe) at IOoC (or while maintaining gentle reflux; while keeping inner temperaturebetween 10oC - 30oC) under N2 (液體滴加到反應(yīng)液中)2.1.1.2: D (10 g, I mole) was added in portions duri

4、ng a period of 1 hr (固體分批加 入到反應(yīng)液中)2.1.1.3: D (10 g, 1 mole) and E (20 mL) were added in turn2.2:To a solution (mixture, suspension or slurry) of A (10 mL, 1 mole) and B (2 g, mole) in C (50mL)2.2.1: was added dropwise a solution of D (10 g, 1 mole) in E (20 mL) with stirring at 10oC(or while maintai

5、ning gentle reflux; while keeping inner temperature between I()C 一 30oC)under N2222: was added D (10 g, I mole) in portions during a period of I hrSentence Template for Notebook and Report Writing VVuXiPharmaTech Co., I-td.Confidential Page 2 of 72.23: were added D (10 g, 1 mole) and E (20 mL) in tu

6、rn2.3:2.3.1: A solution of D (10 g, 1 mole) in E (20 mL) was added dropwise into a solution(mixture or suspension) of A (10 mL, I mole) and B (2 g, mole) in C (50 mL) at 10oC (orwhile maintaining gentle reflux; while keeping inner temperature between 10oC 一 30C) underN22.3.2: D (10 g, 1 mole) was ad

7、ded into a solution (mixture or suspension) of A(l() mL, Imole) and B (2 g, mole) in C (50 mL) in portions2.3.3: D (10 g, I mole) and E (2() mL) were added into a solution (mixture or suspension) ofA (lOmL, I mole) and B (2 g, mole) in C (50 mL) in turn2.4:2.4.1: A solution of BuLi or BH3/THF (10 mL

8、, I mole, 2.5 M in hexane) was cannulated intoaddition funnel or into a solution A in solvent B2.4.2: A solution of BuLi or BHVTHF (10 mL, 1 mole, 2.5 M in hexane) was added into asolution of A in solvent B via cannula, dropping funnel or syringe over a period of hrs Part 3:反應(yīng)3.1:無溶劑反應(yīng)A (1 g, 1 mol)

9、 and B (1 g, 1 mol) were dissolved in solvent C, evaporated to dryness andheated for x hours at x oC3.2:催化昴的反應(yīng)A (2() mL, 142 mmol) and catalytic amount (a trace amount or two drops) of B were addedinto a solution of C (4.549 g, 46.4 mmol) in D( 120mL) at 0(C3.3:悶罐反應(yīng)或封管反應(yīng)A solution of A(x g, x mol) i

10、n methanol (x mL) saturated with NHs(or other gas such as: CO,CO2, H2S) was stirred under 50 Psi at x oC for x hours in a 50 mL of sealed tube or autoclave Sentence Template for Notebook and Report Writing WuXiPharmaTcch Co., T.td.Confidential Page 3 of 73.4:有氣體參與的反應(yīng)3.4.1: A solution of A (x g, x mo

11、l) in methanol (x mL) saturated with HCI was stirred at x C.3.4.2: Ozone was bubbled into a solution of A (x g, x mol) in MeOH (x mL) at x oC for 15minutes. After excess O3 was purged by N2, Me2S (x mL) was added at x oC3.4.3: Gas was bubbled into a solution of A (x g, x mol) and B (x g, x mol) in s

12、olvent C(xmL) at x oC for x hours.3.5:混合溶劑參與的反應(yīng)3.5.1: To a solution of A (x g, x mol) in a mixture of solvent B (mL) and solvent C (x mL) (ora mixed solvent of B and C) was added D (x g, x mol) at x C, the reaction mixture wasallowed to stir (reflux or heat) for x hrs.3.5.2: To a solution of A (x g,

13、 x mol) in 1(): I aqueous acetone (x mL) was added B (x g，Xmol) followed by addition of C (x g, x mol), the reaction mixture was allowed to stir (refluxor heat) for x hrs.3.6:分水器分水的反應(yīng)3.6.1: A (x g, x mol) and B (x g, x mol) in benzene or toluene (x mL) were refluxed for xhours with azeotropical remo

14、val of water.362; A mixture of A, B and TsOHHO (56.91 g, 0.3 mol) in toluene (400 mL) was heated toreflux and remove water by Dean-Stark trap.3.7:氫化反應(yīng)To a solution of A (x g, x mol) in EtOH (x mL) was added Pd-C or Ra-Ni or Pd(OH)2/C(10%,x g) under N2. The suspension was degassed under vacuum and pu

15、rged with H2 several times3.7.1: The mixture was stirred under H2(x psi) at x C for x hours就化瓶或高丿 k 釜3.7.2: The mixture was stirred under H2 balloon at x C for x hours. | 常壓氫化如氣球 反應(yīng)3.7.3: A mixture of A (x g, x mol) and Ra-Ni (x g) in EtOH (x mL) was hydrogenated under50 Psi of hydrogen pressure for

16、 x hours at room temperatureSentence Template for Notebook and Report Writing VVuXiPharmaTech (x., Ltd.Confidential Page 4 of 7Part 4:反應(yīng)條件或過程描述4.1: The reaction mixture (solution or suspension) was stiiTed at 5oC for 2 hrs and then kept atroom temperature (or ambient temperature) for another 2 hrs (

17、or overnight)4.2: The reaction mixture (solution or suspension) was refluxed (heated to reflux) or heated at60oC for 2 hrs (or overnight)4.3: The reaction mixture (solution or suspension) was allowed to reflux (or heat to reflux) for2 hrs (or overnight)4.4: The reaction mixture (solution or suspensi

18、on) was allowed to warm to temperature during2 hrs and reflux (or heat to reflux) for 2 hrs (or overnight)Part 5:反應(yīng)監(jiān)測5.1: Taking sample from the reaction mixture (solution or suspension) by dropping tube orsyringe. After workup, check the reaction via TLC, LC-MS or HPLC etc.(預(yù)處理) 5.2:反應(yīng)狀態(tài)或終點描述5.2.1:

19、 The reaction was complete (incomplete or messy) detected (determined or confirmed)by TLC (PE/EtOAc 4:1), LC-MS, HPLC or NMR5.2.2:TLC (PE:EtOAc= l:l)or HPLC (107757-088-1)showed or indicated that the reactionwas complete.5.2.3: TLC (PE:EtOAc= 1:1) or HPLC (107757-088-1) showed the starting material

20、wasconsumed completely5.2.4: TLC (PE:EA=I: I) or HPLC (107757-088-1) showed the reaction didnt work at all ormost of starting material was still remained.5.2.5: The starting material was consumed completely, but no desired compound was detectedor determined by MS(106657-078-1) or LC-MS (106657-078-1

21、).5.2.6: Several spots were shown on TLC5.2.7: Only a trace amount of desired compound was delected by MS (106657-078-1) orLC-MS (106657-078-1) or HPLC (106657-078-1) or TLC (PE:EtOAc= 1:1).52& The desired compound could not be isolated, separated or purified by chromatographyor prep. HPLC due to po

22、or yield or poor solubility.Sentence Template for Notebook and Report Writing VVuXiPliarinaTcdi Co., LtdConfidential Page 5 of 75.2.9:iH NMR (106675-010-2) or MS confiitned the obtained (or isolated) compound is notthe desired compound. The reaction was failedPart 6:反應(yīng)淬滅6：An aqueous solution of A (1

23、() mL) was added dropwise into the reaction mixture once thereaction mixture (solution or suspension) was allowed to warm (or cool) to -5(C or roomtemperature (ambient temperature).6.2: The hot (or cold) reaction mixture (solution or suspension) was poured into water (icewater) or poured onto ice.6.

24、3: The reaction mixture (solution or suspension) was concentrated (distilled) under reducedpressure (in vacuum) or evaporated to remove McOH (THF; DMF etc.) or excess SOC12(reagent). Then the reaction residue (or the residual) was diluted with solvent and poured intowater (ice water) or poured onto

25、ice.Part 7:分液提取7.1: The residue was partitioned between ethyl acetate (100 mL) and IN aq. HC1 (50 mL).The separated organic layer was washed with waler, dried over (Na2SO4 or MgSO4) andevaporated to dryness7.2: After quenching the reaction, the reaction mixture was poured into separatory funnel ands

26、eparated 7.3: The aqueous layer (or phase) was extracted with organic solvent (40 mL) twice (orXtimes). The combined organic layers were (or the organic layers were combined and) washedwith an aqueous solution of A (50 mL) or water and dried over Na2SO4 or MgSO4. 7.4: The combined aqueous layers wer

27、e extracted with solvent (40 mL) twice (or X times) toremove neutral impurities The aqueous phase was acidified (or basifled) with aqueous HCI(or NaHCO3) till PH = X and extracted with organic solvent.7.5: The combined organic layers were (or the organic layers were combined and) washedwith an aqueo

28、us solution of A (5() mL) or water and dried over Na2SO4 or MgSO4. Sentence Template for Notebook and Report Writing WuXiPharmaTedi Co., Ltd.Coii/ideiitial Page 6 of 7Part 8:濃縮蒸發(fā)8.1: After fillration via filter paper or Celite pad, the organic layer (or extract) was concentrated under reduced pressu

29、re (or in vacuum) or evaporated to dryness to provide(afford; give or yield) an oil (or foam) (which solidified on standing) or a white solid. 8.2: The organic layer (or extract) was filtered and concentrated under reduced pressure (or invacuum) or evaporated to dryness to provide (afford or give) A

30、 (10 g, 0.5 mole) an oil (orfoam) (which solidified on standing) or a white solid8.3: After removal of solvent by evaporation or concentration, A (10 g, 0.5 mole) was obtained (or prepared) an oil (or foam) (which solidified on standing) or a white solid. 8.4: The extract in CH2CI2 was evaporated to

31、 dryness and then swapped with toluene toremove residual CH2CI2Part 9:兒種常見的后處理描述9.1: The reaction mixture or solution was concentrated to dryness適用 于反應(yīng)液不需要quench9.2: After the reaction mixture was cooled to 0 C, the reaction mixture was quenched byaddition of x mL of H2O, followed by x mL of 15% aqu

32、eous NaOH. After being stirred atroom temperature for x hour, the solid was removed by filtration (or the mixture was filteredlliroughCelite pad to remove by-product). The filtrate was concentrated to dryness to givecrude product. LiAlH4反應(yīng)的經(jīng)典后處理9.3: The mixture was diluted with water (x mL), neutral

33、ized with solid K2CO3 until no CO2was evolved.適用于酸性反應(yīng)液的后處理9.4: The suspension was filtered through a pad of Celite or silica gel and the pad or filter cakewas washed with EtOH (x mLXx). The combined filtrates were concentrated to dryness togive product (x g, x%) as.適用氫化反應(yīng)的后處理，或者難丁過濾的反應(yīng)液的后 處理，但要注意的是這

34、里需要的是濾液而不是固體才能添加助濾劑9. 5: The reaction mixture was poured into x mL of ice-water carefully and the organic layer orphase was separated.產(chǎn)物在有機相里9. 6: The reaction mixture was poured into x mL of ice-water carefully and the aqueous phasewas washed with Et2O (x mLXx)產(chǎn)品在水相and acidified with IN HC1 to pH=3

35、. TheSentence Template for Notebook and Report Writing WuXiPharmaTech Co., Ltd.Confidential Page 7 of 7resulting precipitate was collected by filtration or the resulting solution was extracted with EA(x mLXx).9. 7: The reaction mixture was filtered and the filter cake was washed with x mL of solvent,dried in vacuum to give or afford product.這里需