HRID1658029

反应详情

EQUATION

反应方程式

HRID 1658029 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Hydrogen sulfide (0.75 g) is passed into a cold (ice-bath) solution of p-methoxybenzyl α-amino-dimethylphosphonoacetate (6.06 g) in anhydrous methanol (5 ml). Hydrogen cyanide (0.53 g) is added and the ice-bath is removed. After standing overnight, the reaction mixture is added to water (50 ml) and extracted with ether (3 × 20 ml). The combined extracts are dried with magnesium sulfate, filtered, and evaporated in vacuo to dryness. The residue is chromatographed on silicon gel, affording p-methoxybenzyl α-thioformamido-dimethylphosphonoacetate.

WORKUP

后处理

  1. customthe ice-bath is removed
  2. additionthe reaction mixture is added to water (50 ml)
  3. extractionextracted with ether (3 × 20 ml)
  4. dry with materialThe combined extracts are dried with magnesium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo to dryness
  7. customThe residue is chromatographed on silicon gel