HRID355213

反应详情

EQUATION

反应方程式

HRID 355213 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,6-Lutidine (2.14 g., 20 mmole) was added to a solution of p-nitrobenzyl 2-(4-acetylthio-2-oxo-1-azetidinyl)-2-chloroacetate (5.9 g., 16 mmole) and triphenylphosphine (5.8 g., 22 mmole) in dioxane (80 ml.). The solution was kept at 55° for 18 hours and then concentrated on a rotary evaporator. The residue was partitioned between brine and ethyl acetate and the organic phase was washed with brine, dried and concentrated. The residue was purified by chromatography over silica gel (ethyl acetate:petroleum ether, 1:2 v/v) to give 4.64 g. (48%) of the title ester.

WORKUP

后处理

  1. concentrationconcentrated on a rotary evaporator
  2. customThe residue was partitioned between brine and ethyl acetate
  3. washthe organic phase was washed with brine
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by chromatography over silica gel (ethyl acetate:petroleum ether, 1:2 v/v)
  7. customto give 4.64 g