反応 #65134

反応方程式

4-chlorobutyryl chloride

10,11-dihydrodibenzo[b,e][1,4]diazepin-11-one

→

title compound

5- (4-Chlorobutyryl)-10,11-dihydrodibenzo [b,e][1,4]diazepin-11-one

溶媒

acetone

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度under reflux for 8 hours
3. 3
   その他evaporated
4. 4
   その他The residue was purified by chromatography on silica
5. 5
   その他evaporated
6. 6
   その他the residue triturated with hexane/dichloromethane

実験手順

A mixture of 4-chlorobutyryl chloride (3.5 g) and 10,11-dihydrodibenzo[b,e][1,4]diazepin-11-one (4.2 g) (J. Med. Chem., 1963, 6, 767) in acetone (90 ml) was heated under reflux for 8 hours and evaporated. The residue was purified by chromatography on silica using hexane plus 0-100% dichloromethane as eluant. Appropriate fractions were combined and evaporated and the residue triturated with hexane/dichloromethane to give the title compound as a colourless solid, 1.62 g (26%), m.p. 151°-152° C.

出典