反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
To 15 g. 4-[15-(trifluoromethyl)pentadecylamino]-benzoic acid in 200 ml. warm chloroform is added a solution of 15 g. of sodium carbonate in 150 ml. water. To the vigorously stirred solution is added 10 g. carbobenzyloxy chloride. After 2 hours stirring at 40° C., the layers are separated, washed three times with 1 N hydrochloric acid, dried, and evaporated to an oil. The oil is dissolved in 300 ml. toluene, treated with 15 ml. thionyl chloride and the solution is refluxed for 5 hours. The solvents are evaporated and the residue is dissolved three times in toluene, evaporating each time, ultimately to yield 4-[N-carbobenzyloxy-15-(trifluoromethyl)pentadecylamino]benzoyl chloride as a viscous, orange oil.
WORKUP
后处理
- additionTo the vigorously stirred solution is added 10 g
- customthe layers are separated
- washwashed three times with 1 N hydrochloric acid
- customdried
- customevaporated to an oil
- dissolutionThe oil is dissolved in 300 ml
- additiontoluene, treated with 15 ml
- temperaturethionyl chloride and the solution is refluxed for 5 hours
- customThe solvents are evaporated
- dissolutionthe residue is dissolved three times in toluene
- customevaporating each time