HRID2395047

反应详情

EQUATION

反应方程式

HRID 2395047 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-30 °C

PROCEDURE

实验过程

3-tertbutoxycarbonyl-6-methyl-2(1 H)-pyridinone (1.49 g, J. Het. Chem., 1981, 18, 1611) was added to a THF (20 ml) solution of lithium diisopropylamide (14.3 mmol, prepared by the standard method) and stirred under argon, at -30° C., for 2.5 hours. 2-Benzyloxybenzyl bromide (2 g, prepared as described in Example 1) in THF (10 ml) was added and the mixture stirred, at -30° C., for 1 hour, then warmed to ambient temperature. The mixture was poured into saturated aqueous ammonium chloride (200 ml) and extracted with dichloromethane. The solvent was evaporated and crystallised from isopropranol. There was thus obtained 6-(2-[2-benzyloxyphenyl)ethyl]-3-tertbutoxycarbonyl-2(1 H)-pyridinone (1.85 g) m.p. 146°-147° C.

WORKUP

后处理

  1. customprepared by the standard method) and
  2. stirringthe mixture stirred, at -30° C., for 1 hour
  3. temperaturewarmed to ambient temperature
  4. extractionextracted with dichloromethane
  5. customThe solvent was evaporated
  6. customcrystallised from isopropranol