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1、最全有机实验记录英文描述总结一、加料过程常用表述1. 添加试剂2. 催化量的3. 气体保护4. 通入气体5. 通过双针头导管加料6. 通过注射器加料二、反应过程常用表述1. 反应检测2. 放置过夜3. 甲苯 / 乙醇带水4. 氢化反应5. 分水器6. 反应放热7. 微波反应三、后处理过程常用表述1. 过滤2. 淬火3. 磨碎4. 在两相中分开5. 静止固化6. 在冻干机冻干7. 纯化过柱制备 HPLC 纯化制备 TLC 纯化重结晶8. 调 pH9. 萃取10. 浓缩11. 干燥干燥真空干燥四、部分常见反应现象描述1. 加料放热2. 反应过程中或者降温有固体析出3. 加料不溶解4. 加热溶解5.
2、 反应变粘稠 / 变色五、特殊结果叙述1. 无进一步处理2. 统一和其他批次一起后处理3. 检测条件，不需要后处理六、一些易错写法一、加料过程常用表述1. 添加试剂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. 气体保护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. 通入气体
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. 通过双针头导管加料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. 通过注射器加料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、反应过程常用表述1. 反应检测After 1 h, TLC analysis (CH2 Cl2/ hexane 3:1) showed the complete consumption of compound 15.2.
8、放置过夜The mixture was left standing overnight.3. 甲苯 / 乙醇带水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. 氢化反应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. 反应放热The reaction was exothermic.7. 微波反应The sealed vial was irradiated in the microwave on aBiotage Smith Synthesis at 150oC for 10 min.三、后处理过程常用表述1. 过滤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. 在两相中分开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. 静止固化The crude product was purified by prep-HPLC to givecompound4 as colorless thick oil,which was solidified on standing.6. 在冻干机冻干The white s
13、olid was re-crystallized from water, driedby hyophilization to give a white solid.7. 纯化过柱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 with (CH2Cl2 / MeOH 20:1 10:1 5:1)to give the compound8(0.282 g,51%) as a white solid.制备 HPLC纯化be purified by prep-HPLC to afford/give/yield制备 TLC纯化be purified by prepare TL
