HRID1438786

反应详情

EQUATION

反应方程式

HRID 1438786 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

2,2,2-Trichloroethyl 2-bromomethyl-2-methyl-6-(2-phenylacetamido)-penam-3-carboxylate (1.10 g) was dissolved in methylene chloride (12 ml) and to this solution was added methanol (3 ml). And to the solution was added silver fluoroborate (0.45 g) under stirring under cooling at -10° C and the mixture was stirred for 2 hours at the same temperature. After the reaction was completed, the reaction mixture was filtered and the filtrate was washed with sodium bicarbonate aqueous solution and then with water, dried over magnesium sulfate and thereafter concentrated. The residue was subjected to column chromatography on silica gel (25 g) and eluted with chloroform. The eluate was seprated into fractions of about 20 ml and the first and second fractions were collected. After distilling off the solvent, the residue was dried to give oily 2,2,2-trichloroethyl 2-methoxymethyl-2-methyl-6-(2-phenylacetamido)penam-3-carboxylate.

WORKUP

后处理

  1. stirringthe mixture was stirred for 2 hours at the same temperature
  2. filtrationthe reaction mixture was filtered
  3. washthe filtrate was washed with sodium bicarbonate aqueous solution
  4. dry with materialwith water, dried over magnesium sulfate
  5. concentrationconcentrated
  6. washeluted with chloroform
  7. customthe first and second fractions were collected
  8. distillationAfter distilling off the solvent
  9. customthe residue was dried