HRID1388090

反应详情

EQUATION

反应方程式

HRID 1388090 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 5.18 g. portion of diphenylmethyl 2-(4-chloro-3-phenoxyacetamido-2-oxo-1-azetidinyl)-3-methyl-3-butenoate was dissolved in 200 ml. of methyl formate, and 1.71 ml. of t-butyl hypochlorite was added. The mixture was stirred at room temperature for 16 hours. It was then evaporated under vacuum to obtain a white foam, which was taken up in ethyl acetate and washed three times with water. The organic layer was then decolorized with activated carbon, dried over magnesium sulfate, and evaporated to a white foam. The foam was taken up in 100 ml. of dry diethyl ether, from which 1.12 g. of the desired product was obtained in crystalline form. The product was analyzed by infrared in chloroform, showing maxima at 1795, 1745 and 1695 cm-1 ; a second spectrum in methanol showed maxima at 1775, 1740 and 1695 cm-1. NMR analysis on a 100 megacycle instrument in CDCl3 showed the following δ values. 4.24(s); 4.63(s); 5.73(center of q); 6.2(d); 5.09(s); 5.33(s); 5.5(s)

WORKUP

后处理

  1. customIt was then evaporated under vacuum
  2. customto obtain a white foam, which
  3. washwashed three times with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated to a white foam