HRID2296589

反应详情

EQUATION

反应方程式

HRID 2296589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

165 mg of bis-(2-methylthioethyl)-amine (Example 8b) is dissolved in 20 ml of acetonitrile and mixed with 174 μl of diisopropylethylamine. 92.7 μl of bromoacetic acid methyl ester, dissolved in 20 ml of acetonitrile, is added in drops under a cover-gas atmosphere, and the batch is stirred for 18 hours at room temperature. The acetonitrile is drawn off, the residue is taken up with methylene chloride and washed twice with saturated sodium bicarbonate solution. The organic phase is dried with sodium sulfate and concentrated by evaporation, and the residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol: Yield 183 mg=77% of theory.

WORKUP

后处理

  1. additionis added in drops under a cover-gas atmosphere
  2. washwashed twice with saturated sodium bicarbonate solution
  3. dry with materialThe organic phase is dried with sodium sulfate
  4. concentrationconcentrated by evaporation
  5. customthe residue is purified by chromatography with the mobile solvent system of methylene chloride/methanol