HRID1255972

反应详情

EQUATION

反应方程式

HRID 1255972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Compound 29a (0.035 gram, 0.076 mmol) was dissolved in dichloromethane (4.3 ml) and triethylamine (0.032 gram, 3.82 mmol) was added to the resulting solution. Methanesulfonyl chloride (MsCl, 0.025 gram, 0.022 mmol) was then added and the resulting mixture was stirred at room temperature for 3 hours. The mixture was thereafter extracted twice with CH2Cl2, washed with brine and dried over sodium sulfate. The crude residue was purified by silica gel column chromatography, using a mixture of 2% methanol in dichloromethane as eluent, to give Compound 32a (0.012 gram, 29% yield).

WORKUP

后处理

  1. extractionThe mixture was thereafter extracted twice with CH2Cl2
  2. washwashed with brine
  3. dry with materialdried over sodium sulfate
  4. customThe crude residue was purified by silica gel column chromatography
  5. additiona mixture of 2% methanol in dichloromethane as eluent