HRID1761236

反应详情

EQUATION

反应方程式

HRID 1761236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of N-[(5S)-3,9,10,11-tetramethoxy-6,7-dihydro-5H-dibenzo[a,c]cyclohepten-5-yl]-2-[2-(butoxycarbonylamino)acetylamino]acetamide (0.9 g ; 0.64 mmol) in dichloromethane (6 ml) was treated with TFA (6 ml) at ambient temperature for 0.5 hour. After evaporation to dryness, the residue was neutralised to pH 6.5 with solid sodium hydrogen carbonate and purified on reverse phase silica eluting with a gradient of 30-40% methanol/ammonium carbonate buffer (2 g/l, pH 7). The appropriate fractions were evaporated to dryness and triturated in ether to give the title compound.

WORKUP

后处理

  1. customAfter evaporation to dryness
  2. custompurified on reverse phase silica eluting with a gradient of 30-40% methanol/ammonium carbonate buffer (2 g/l, pH 7)
  3. customThe appropriate fractions were evaporated to dryness
  4. customtriturated in ether