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
PROCEDURE
实验过程
A solution of 184.3 g 2-chloro-N-cyclopropylmethyl-N-[2-(3-phenyl-1H-indol-2-yl)ethyl]acetamide in 1843 ml methylene chloride is added dropwise under vigorous stirring to a suspension of 17.9 g N-benzyltributyl-ammoniumbromide in 1843 ml methylene chloride and 921 ml 30% sodium hydroxide. The mixture is stirred for further 10 minutes and diluted with 1 l water. The organic phase is separated, washed with water, dried and evaporated to dryness. The residue is dissolved in 500 ml boiling ethanol, cooled and treated with 500 ml ether. The resulting cristalline precipitate is filtered off, washed with ethanol/ather (1:1) and then ether to give 2,3-dihydro-3-cyclopropylmethyl-11-phenyl-1H-[1,4]diazepino[1,7-a]indol-4(5H)-one, m.p. 149°-150°.
WORKUP
后处理
- customThe organic phase is separated
- washwashed with water
- customdried
- customevaporated to dryness
- dissolutionThe residue is dissolved in 500 ml
- temperaturecooled
- additiontreated with 500 ml ether
- filtrationThe resulting cristalline precipitate is filtered off
- washwashed with ethanol/ather (1:1)