HRID543260

反应详情

EQUATION

反应方程式

HRID 543260 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution containing 60 g (0.30 mol) of N-cyclopentylglycine t- butyl ester and 75 ml (0.54 mol) of triethylamine in 200 ml of methylene chloride at 0° C. was added dropwise a solution of 54 g (0.30 mol) of 3-acetylthio-2-methylpropanoyl chloride in 250 ml of methylene chloride. After the reaction mixture was stirred at room temperature overnight, it was filtered and concentrated in vacuo. The residue was taken up in ethyl acetate and wasned once with saturated aqueous NaHCO3, once with brine, three times with 5% aqueous HCl, once with brine, and five times with saturated aqueous NaHCO3. The organic phase was dried over MgSO4, filtered, and concentrated in vacuo to yield 80.1 g (78%) of N-(3-acetylthio-2-methylpropanoyl)-N-cyclopentylglycine t-butyl ester as an oil which crystallized on standing.

WORKUP

后处理

  1. filtrationit was filtered
  2. concentrationconcentrated in vacuo
  3. dry with materialThe organic phase was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo