N-[3-（二甲基氨基）丙基]十四烷酰胺

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2.0 g. (0.0196 moles) of 3-dimethylaminopropylamine in 40 ml chloroform was added dropwise to an ice cold chloroform solution (50 ml) of myristoyl chloride (4.17 g., 0.0169 moles). After addition, the ice bath was removed and the solution was stirred for 2 hours. A 25 ml aqueous sodium bicarbonate solution was added and stirred for 30 minutes. The organic layer was then washed with 30 ml aqueous sodium bicarbonate/sodium chloride solution and dried with magnesium sulfate. The solution was concentrated in vacuo and the amide was recrystallized in ethyl acetate to yield 3.29 g. (0.0105 moles, 62.3%) of the subject compound. After addition the ice bath was removed A 25 ml aqueous sodium bicarbonate solution was added stirred for 30 minutes The organic layer was then washed with 30 ml aqueous sodium bicarbonate/sodium chloride solution dried with magnesium sulfate The solution was concentrated in vacuo the amide was recrystallized in ethyl acetate to yield 3.29 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2.0 g. (0.0196 moles) of 3-dimethylaminopropylamine in 40 ml chloroform was added dropwise to an ice cold chloroform solution (50 ml) of myristoyl chloride (4.17 g., 0.0169 moles). After addition, the ice bath was removed and the solution was stirred for 2 hours. A 25 ml aqueous sodium bicarbonate solution was added and stirred for 30 minutes. The organic layer was then washed with 30 ml aqueous sodium bicarbonate/sodium chloride solution and dried with magnesium sulfate. The solution was concentrated in vacuo and the amide was recrystallized in ethyl acetate to yield 3.29 g. (0.0105 moles, 62.3%) of the subject compound. After addition the ice bath was removed A 25 ml aqueous sodium bicarbonate solution was added stirred for 30 minutes The organic layer was then washed with 30 ml aqueous sodium bicarbonate/sodium chloride solution dried with magnesium sulfate The solution was concentrated in vacuo the amide was recrystallized in ethyl acetate to yield 3.29 g

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2.0 g. (0.0196 moles) of 3-dimethylaminopropylamine in 40 ml chloroform was added dropwise to an ice cold chloroform solution (50 ml) of myristoyl chloride (4.17 g., 0.0169 moles). After addition, the ice bath was removed and the solution was stirred for 2 hours. A 25 ml aqueous sodium bicarbonate solution was added and stirred for 30 minutes. The organic layer was then washed with 30 ml aqueous sodium bicarbonate/sodium chloride solution and dried with magnesium sulfate. The solution was concentrated in vacuo and the amide was recrystallized in ethyl acetate to yield 3.29 g. (0.0105 moles, 62.3%) of the subject compound. After addition the ice bath was removed A 25 ml aqueous sodium bicarbonate solution was added stirred for 30 minutes The organic layer was then washed with 30 ml aqueous sodium bicarbonate/sodium chloride solution dried with magnesium sulfate The solution was concentrated in vacuo the amide was recrystallized in ethyl acetate to yield 3.29 g

实验步骤: 投料: 加入SM1，加入甲苯，加入SM2，160℃反应，分水器分水，反应2h，然后降温至100℃反应过夜，然后后面升温至160℃，反应7h

实验步骤: 投料: 加入SM1，加入甲苯，加入SM2，130℃反应，分水器分水，反应7h，然后后面升温至160℃，反应7h，100℃反应15h，160℃反应5h

实验步骤: 投料: 加入SM1，加入DCM，氮气置换三次，加入氯化亚砜，升温至45℃反应，反应过夜后，反应完全，反应液直接浓缩，然后加入SM2和三乙胺，RT反应，反应完后，反应液用碱水洗，分相，有机相浓缩，有机相用pe打浆（但是没有得到干净的产品），然后用PE/EA打浆（得不到干净的产品）

实验步骤: 投料: 加入SM1，加入DCM，氮气置换三次，加入氯化亚砜，RT反应，后升温至45℃反应，反应液直接浓缩，然后加入SM2和三乙胺，RT反应，反应完后，反应液用酸水和碱水洗，然后用EA打浆（但是没有得到干净的产品），然后用甲叔醚打浆（得不到干净的产品）

实验步骤: 投料: A：加入SM1，DCM，加入EDCI，加入DMAP，加入三乙胺，RT反应过夜，然后50℃反应 B：加入SM1，DCM，加入HATU，加入DMAP，加入三乙胺，RT反应过夜，然后50℃反应

实验步骤: 辅助生产: 辅助生产\n投料: 在10L反应釜中，加入SM1（1.41kg），加入DCM（7.42kg），氮气置换三次，加入氯化亚砜（1.44kg），升温至40℃反应，反应5h，反应完后，反应液直接浓缩，然后加入SM2（1.25kg），DCM（7.9kg），然后降温至0-10℃，滴加A1，滴完后，回至RT反应，反应1h后送GC中控，反应完后，反应液过滤，然后滤液用2800ml水洗，然后分相，有机相用2100ml水洗，合并有机相，有机相浓缩，浓缩完后，加入乙酸乙酯（13.5kg），活性炭（190g），升温至60℃搅拌1h，然后降温至25℃搅拌1h，然后过滤，滤液浓缩，浓缩液加入5.8kg石油醚50℃重结晶，溶清后降温至0-5℃搅拌1h，然后过滤，固体烘干，颜色偏黄。重新用300g活性炭，13.5kg乙酸乙酯搅拌过夜，然后过滤，固体浓缩干大部分，然后38℃真空干燥 \n辅助生产: 辅助生产\n辅助生产: 辅助生产

实验步骤: 01-24 14:33: 加入SM1（10g），加入DCM（40ml），氮气置换三次，加入氯化亚砜（10.4g），升温至45℃反应，反应过夜，反应完后，反应液直接浓缩，然后加入SM2（8.9g），DCM（22ml），然后降温至0-10℃，滴加A1（DCM22ml），滴完后，回至RT反应，反应1h后送GC中控，反应完后，反应液过滤，然后滤液用20ml水洗，然后分相，有机相用15ml水洗，合并有机相，有机相浓缩

实验步骤: 投料: 加入SM1（1g），加入DCM（4ml），氮气置换三次，加入氯化亚砜（0.68g），升温至45℃反应，反应过夜，补加0.3eq氯化亚砜，反应4h，补加0.4eq氯化亚砜，反应完全

实验步骤: 投料: 加入SM1（100g），加入DCM（400ml），氮气置换三次，加入氯化亚砜（156.7g），升温至45℃反应，反应过夜，反应完后，反应液直接浓缩，然后加入SM2（134.2g），DCM（270ml），然后降温至0-10℃，滴加A1（DCM270ml），滴完后，回至RT反应，反应1h后送GC中控，反应完后，反应液过滤，然后滤液用200ml水洗，然后分相，有机相用150ml水洗，合并有机相，有机相浓缩，浓缩完后用500mlPE重结晶（60℃），然后降温至0-5℃，保温30min，过滤，固体用10%活性炭吸附过滤