HRID356164
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
- 140 °C
PROCEDURE
实验过程
A suspension of (3aR*,10aS*)-4-(aminoacetyl)-9-benzyl-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta-[e][1,4]diazepin-10(1H)-one (490 mg, 1.4 mmol) and 4-fluorophthalic acid anhydride (233 mg, 1.4 mmol) in xylene (3 mL) was stirred for 30 minutes at 140° C. The reaction mixture was left standing for cooling at room temperature, to which was added hexane (5 mL). The resulting solid was collected by filtration, followed by recrystallization from dichloromethane-hexane to give 436 mg (yield 62%) of the titled compound, m.p. 235°-236° C.
WORKUP
后处理
- waitThe reaction mixture was left
- temperaturefor cooling at room temperature, to which
- filtrationThe resulting solid was collected by filtration
- customfollowed by recrystallization from dichloromethane-hexane