HRID355679

反应详情

EQUATION

反应方程式

HRID 355679 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In an atmosphere of argon, 30 ml of methanol solution containing 2.03 g of the compound of Example 39 was mixed with 500 mg of palladium black and stirred for 3 days to effect hydrogenation. Then, 1 g of activated carbon was added and the mixture was filtered. The filtrate was evaporated under reduced pressure and then the residue was subjected to silica gel column chromatography and elution was carried out with a series of mixed solutions of chloroform:methanol=40:1 and 20:1 and chloroform:methanol:concentrated aqueous ammonia=300:10:1 and 100:10:1 in that order to obtain 120 mg of methyl 2-benzyloxycarbonylamino-3-[5-(1-hexahydroazepinylmethyl)-2-thienyl]propionate.

WORKUP

后处理

  1. additionThen, 1 g of activated carbon was added
  2. filtrationthe mixture was filtered
  3. customThe filtrate was evaporated under reduced pressure
  4. washthe residue was subjected to silica gel column chromatography and elution