最全有機(jī)實驗記錄英文描述總結(jié)

1、最全有機(jī)實瞼記錄英文描述總結(jié)目錄 TOC o 1-5 h z HYPERLINK l bookmark4 o Current Document .加料過程常用表述2 HYPERLINK l bookmark6 o Current Document 1.添加試劑2催化量的2 HYPERLINK l bookmark8 o Current Document 氣體保護(hù)3 HYPERLINK l bookmark10 o Current Document 通入氣體3 HYPERLINK l bookmark12 o Current Document 通過雙針頭導(dǎo)管加料3 HYPERLINK l boo

2、kmark14 o Current Document 通過注射器加料3 HYPERLINK l bookmark16 o Current Document .反響過程常用表述3 HYPERLINK l bookmark18 o Current Document 1.反響檢測32.放置過夜33.甲苯/乙醇帶水3 HYPERLINK l bookmark24 o Current Document 4.氫化反響4 HYPERLINK l bookmark26 o Current Document 5.分水器4 HYPERLINK l bookmark28 o Current Document 6.反

3、響放熱4 HYPERLINK l bookmark30 o Current Document 7.微波反響4 HYPERLINK l bookmark32 o Current Document .后處理過程常用表述4 HYPERLINK l bookmark34 o Current Document 1.過濾4 HYPERLINK l bookmark36 o Current Document 2.淬火4 HYPERLINK l bookmark38 o Current Document 3.磨碎4 HYPERLINK l bookmark40 o Current Document 4.在兩相

4、中分開5 HYPERLINK l bookmark42 o Current Document 5.靜止固化5 HYPERLINK l bookmark44 o Current Document 6.在凍干機(jī)凍干57.純化53. 7. 1.過柱53. 7. 2.制備HPLC純化53.7.3.制備TLC純化53. 7. 4.重結(jié)晶53. 8.調(diào) pH5 HYPERLINK l bookmark52 o Current Document 3. 9.萃取6第1頁共7頁 TOC o 1-5 h z HYPERLINK l bookmark54 o Current Document 3. 10.濃縮63.

5、 11.干燥6 HYPERLINK l bookmark59 o Current Document 11. 1.干燥611.2.真空干燥6 HYPERLINK l bookmark61 o Current Document 4.局部常見反響現(xiàn)象描述6 HYPERLINK l bookmark63 o Current Document 1.加料放熱6 HYPERLINK l bookmark65 o Current Document 2.反響過程中或者降溫有固體析出6 HYPERLINK l bookmark67 o Current Document 3.加料不溶解6 HYPERLINK l b

6、ookmark69 o Current Document 4.加熱溶解6 HYPERLINK l bookmark71 o Current Document 5.反響變粘稠/變色7 HYPERLINK l bookmark73 o Current Document 5.特殊結(jié)果表達(dá)7 HYPERLINK l bookmark75 o Current Document 1. 無進(jìn)一步處理7 HYPERLINK l bookmark77 o Current Document 2.統(tǒng)一和其他批次一起后處理7 HYPERLINK l bookmark79 o Current Document 一些易錯

7、寫法7.加料過程常用表述1.添加試劑To a mixture (suspension / solution / slurry) of compound 12 (487 mg, 1 mmol) and o-plenylenediamine (648 mg, 6 mmol) in CH2c1 (15 mL) being cooled to 0 was added the DCC (226 mg, 1.1 mmol).Anhydrous lithium iodide (1.38 g, 10.3 mmol) was added the five portions (dropwise/ in one p

8、ortion / in portions) to a stirred solution of compound 12(10.93 g, 51.5mmol)inCH2CI2(120mL).A round-bottom flask was charged with compound 3 (1.75 g, 5.27 mmol), LiCI (1.17g, 26.3 mmol), DMSO (100 mL) and H20 (378pL) 1.2.催化量的Et3N (20 mL, 142 mmol) and a catalyticamount of DMAP were added the soluti

9、on of compound 1 (4.549 g, 46.4mmol) in CH2c% (120 mL) at 0第2頁共7頁3.氣體保護(hù)To a stirred -78solution of trimethylsilyacetylene (4.44 g, 45.5 mmol) in THF (10 mL) under Argon wasadded dropwise n-butylithium (1.6 M in hexane, 28.25 mL).通入氣體An ozone-enriched steam of oxygen was bubbled througha cold (-78) s

10、olution of compound 9 (128 mg, 1.409 mmol) in CH2ch (5 mL) untilit turned light blue. The solution was purged with argon at -78for 10 min to remove the excess O3.通過雙針頭導(dǎo)管加料The mixture was added to a solution of compound 2 (3.00 g, 12.8 mmol) in THF (48mL) via cannjiLa over a period of 30 min.A soluti

11、on of compound 29 (100 mg, 0.19 mmol, 1.0 equiv) in dry DMSO (1.5 mL) wascannpLated 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, 0.45 equiv) in dry DMSO (0.5 mL).通過注射器加料To a stirred solution of compou

12、nd 15 (8.61 g, 21.2 mmol)was added a solution ofp-toluenesuLfonicacid (6.0 g) in CH2cvia syringe over 5 min.2 .反響過程常用表述2. 1.反響檢測After 1 h, TLC analysis (CH2CI2/ hexane 3:1) showed the complete consumption of compound 15.2.放置過夜The mixture was left standing overnight.3.甲苯/乙醇帶水Compound A(1.97 g, 6.63 m

13、mol) was coevaporatedwith toluene five times to remove the water.第3頁共7頁The residue was subjected to toluene azeotrope to givethe corresponding acid chloride as brown oil.The aqueous portion was concentrated underreduced pressure followed by azeotropic removal of water with absolute EtOH4.氫化反響A mixtu

14、re 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.分水器A mixture of TsOH.H2O (56.91 g, 0.3 mol) and toluene (400 mL) washeated to reflux to remove water by Dean-Stark trap.6.反響放熱The reaction was

15、exothermic.7.微波反響The sealed vial was irradiated in the microwave on aBiotage Smith Synthesis at 150 for 10 min.3.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 the crude product.淬火The reaction mixture was quenched by the addition of thesaturated

16、aqueous NH4CL3. 3.磨碎The residue was triturated with ether and filtered to afford a white solid.第4頁共7頁3. 4.在兩相中分開The residue was partitioned between ethyl acetate (100mL) and HCI (1 M aq., 50mL). The organic layer was washed with water, dried (MgS04) andevaporated to dryness.Ethyl acetate (100 mL) an

17、d HCI (1 M aq., 50 mL) were added to the residue, and the layers were separated.3. 5.靜止固化The crude product was purified by prep-HPLC to givecompound 4 as colorless thick oil, which was solidified on standing.3. 6.在凍干機(jī)凍干The white solid was re-crystallized from water, driedby hyophilization to give a

18、white solid.3.7.純化3. 7. 1.過柱The crude product was chromatographed on silica gel(CH2CI2 / MeOH 20:1 玲 10:1 玲5:1) to give the compound 8 (0.282 g, 51%) as a white solid.The crude product was purified by column chromatographyon silica gel eluted with (CH2CI2/ MeOH 20:110:l-5:l)to give the compound 8 (0

19、.282 g, 51%) as a white solid.3. 7. 2.制備HPLC純化be purified by prep-HPLC to afford/give/yield3.7.3.制備TLC純化be purified by prepare TLC to afford/give/yield3. 7. 4.重結(jié)晶 recrystallized from3. 8.調(diào) pHThe pH was adjusted to around 9 by progressivelyadding solid NaHCO3The mixture was adjusted to pH 9 with soli

20、d NaHCO3第5頁共7頁3.9.萃取The aqueous layer was extracted with ethyl acetate (100mL x 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11. 1.干燥The organic layer was dried over MgS04,

21、 andconcentrated.11.2.真空干燥The precipitate was filtered and dried in vacuo (in/ undervacumm; under reduced pressure).4.局部常見反響現(xiàn)象描述1.加料放熱A gentle reflux appeared throughout the additionHeat generated during the addition.The temperature was increased from 25 to50 during the addition.反響過程中或者降溫有固體析出Solid was precipitate out after lh reaction.The reaction mixture was cooled to -IOC , and solid was precipitate out.3.加