HRID1658029
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe ice-bath is removed
- additionthe reaction mixture is added to water (50 ml)
- extractionextracted with ether (3 × 20 ml)
- dry with materialThe combined extracts are dried with magnesium sulfate
- filtrationfiltered
- customevaporated in vacuo to dryness
- customThe residue is chromatographed on silicon gel