(完整版)最全有機(jī)實驗記錄英文描述總結(jié)推薦文檔.docx

1、最全有機(jī)實驗記錄英文描述總結(jié)一、加料過程常用表述1. 添加試劑2. 催化量的3. 氣體保護(hù)4. 通入氣體5. 通過雙針頭導(dǎo)管加料6. 通過注射器加料二、反應(yīng)過程常用表述1. 反應(yīng)檢測2. 放置過夜3. 甲苯 / 乙醇帶水4. 氫化反應(yīng)5. 分水器6. 反應(yīng)放熱7. 微波反應(yīng)三、后處理過程常用表述1. 過濾2. 淬火3. 磨碎4. 在兩相中分開5. 靜止固化6. 在凍干機(jī)凍干7. 純化過柱制備 HPLC 純化制備 TLC 純化重結(jié)晶8. 調(diào) pH9. 萃取10. 濃縮11. 干燥干燥真空干燥四、部分常見反應(yīng)現(xiàn)象描述1. 加料放熱2. 反應(yīng)過程中或者降溫有固體析出3. 加料不溶解4. 加熱溶解5.

2、 反應(yīng)變粘稠 / 變色五、特殊結(jié)果敘述1. 無進(jìn)一步處理2. 統(tǒng)一和其他批次一起后處理3. 檢測條件，不需要后處理六、一些易錯寫法一、加料過程常用表述1. 添加試劑To a mixture (suspension / solution / slurry) ofcompound12 (487 mg, 1 mmol) and o-plenylenediamine (648 mg, 6 mmol) inCH2Cl2 (15 mL) being cooled to 0oC was addedthe DCC (226 mg, 1.1 mmol).Anhydrous lithium iodide (1.3

3、8 g, 10.3 mmol) was added the five portions (dropwise/ in one portion / in portions) to a stirred solution of compound 12 (10.93 g, 51.5mmol) in CH2Cl2(120 mL).A round-bottom flask was charged with compound3 (1.75 g, 5.27 mmol), LiCl (1.17 g, 26.3 mmol), DMSO (100 mL) and H2O (378ul)2. 催化量的Et3N (20

4、mL, 142 mmol) and a catalyticamount of DMAP were added the solution of compound 1 (4.549 g, 46.4mmol) in CH2Cl2 (120 mL) at 0oC3. 氣體保護(hù)To a stirred -78oCsolution of trimethylsilyacetylene (4.44 g, 45.5 mmol) in THF (10 mL) under Argon wasadded dropwisen-butylithium (1.6 M in hexane, 28.25 mL).4. 通入氣體

5、oAn ozone-enriched steam of oxygen was bubbled througha cold (-78C) solution of compound 9 (128 mg, 1.409 mmol) in CH2Cl2 (5 mL) untilit turned light blue. Theosolution was purged with argon at -78Cfor 10 min to remove the excess O3.5. 通過雙針頭導(dǎo)管加料The mixture was added to a solution of compound2 (3.00

6、g, 12.8 mmol) in THF (48mL) via cannula over a period of 30 min.A solution of compound 29 (100 mg, 0.19 mmol, 1.0 equiv) in dry DMSO (1.5 mL) wascannulated under Argon to a vigorously stirred mixture of powered potassiumsuperoxide (62 mg, 0.87 mmol, 4.5 equiv) and 18-crown-6-ether (23 mg, 0.087mmol,

7、 0.45 equiv) in dry DMSO (0.5 mL).6. 通過注射器加料To a stirred solution of compound 15 (8.61 g, 21.2 mmol)was added a solution of p-toluenesulfonicacid (6.0 g) in CH2Cl 2via syringe over 5 min.二、反應(yīng)過程常用表述1. 反應(yīng)檢測After 1 h, TLC analysis (CH2 Cl2/ hexane 3:1) showed the complete consumption of compound 15.2.

8、放置過夜The mixture was left standing overnight.3. 甲苯 / 乙醇帶水Compound A(1.97 g, 6.63 mmol) was coevaporatedwith toluene five times to remove the water.The residue was subjected to toluene azeotrope to givethe corresponding acid chloride as brown oil.The aqueous portion was concentrated underreduced press

9、ure followed by azeotropic removal of water with absolute EtOH4. 氫化反應(yīng)A mixture of compound 1 (190 g, 0.88mmol) and Raney Ni (20 g) inethanol (1500 mL) and ethyl acetate (500 mL) was stirred under 1 atm at room temperaturefor an hour.5. 分水器A mixture of TsOH.H 2O (56.91 g, 0.3 mol) and toluene (400 mL

10、) washeated to reflux to remove water by Dean-Stark trap.6. 反應(yīng)放熱The reaction was exothermic.7. 微波反應(yīng)The sealed vial was irradiated in the microwave on aBiotage Smith Synthesis at 150oC for 10 min.三、后處理過程常用表述1. 過濾The mixture was filtered through a Celite pad, and thefiltrate was concentrated to give t

11、he crude product.2. 淬火The reaction mixture was quenched by the addition of thesaturated aqueous NH4Cl.3. 磨碎The residue was triturated with ether and filtered to afforda white solid.4. 在兩相中分開The residue was partitioned between ethyl acetate (100mL) and HCl (1 M aq., 50mL).The organic layer was washed

12、 with water, dried (MgSO4) andevaporated to dryness.Ethyl acetate (100 mL) and HCl (1 M aq., 50 mL) were added to the residue,and the layers were separated.5. 靜止固化The crude product was purified by prep-HPLC to givecompound4 as colorless thick oil,which was solidified on standing.6. 在凍干機(jī)凍干The white s

13、olid was re-crystallized from water, driedby hyophilization to give a white solid.7. 純化過柱The crude product was chromatographed on silica gel(CH2Cl2 / MeOH 20:1 10:1 5:1) to give the compound8 (0.282 g,51%) as a white solid.The crude product was purified by column chromatographyon silica gel eluted w

14、ith (CH2Cl2 / MeOH 20:1 10:1 5:1)to give the compound8(0.282 g,51%) as a white solid.制備 HPLC純化be purified by prep-HPLC to afford/give/yield制備 TLC純化be purified by prepare TLC to afford/give/yield重結(jié)晶recrystallized from8.調(diào) pHThe pH was adjusted to around 9 by progressivelyadding solid NaHCO3The mixture

15、 was adjusted to pH 9 with solid NaHCO39. 萃取The aqueous layer was extracted with ethyl acetate (100mL 4).10. 濃縮The mixture was evaporated to afford the crudeproduct.The mixture was concentrated afford the crude product.The solvent was removed to afford the crude product.11. 干燥干燥The organic layer was

16、 dried over MgSO4, andconcentrated.真空干燥The precipitate was filtered and dried in vacuo (in/ undervacumm; under reduced pressure).四、部分常見反應(yīng)現(xiàn)象描述1. 加料放熱A gentle reflux appeared throughout the additionHeat generated during the addition.ooThe temperature was increased from 25C to50 C during the addition.2

17、. 反應(yīng)過程中或者降溫有固體析出Solid was precipitate out after 1h reaction.oThe reaction mixture was cooled to -10C,and solid was precipitate out.3. 加料不溶解XX was added to the mixture, and the resultingsuspension was stirred for 2hrs.4. 加熱溶解oThe suspension was heated to 90C andstirred until all solid was dissolved.5.反應(yīng)變粘稠 / 變色The reaction mixture became sticky after 2hrsreaction/stirring.After 2hrs stirring, the mixture turned intoblack/brown/gray/yellow/red color.五、特殊結(jié)果敘述1. 無進(jìn)一步處理No further operation2. 統(tǒng)一和其他批次一起后處理The