HRID745415

反应详情

EQUATION

反应方程式

HRID 745415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-nitrobenzyl 7-[2-(2-aminothiazol-4-yl)-2-benzyloxyiminoacetamido]-3-cephem-4-carboxylate (syn isomer, 2.7 g.), 10% palladium carbon (1 g.), acetic acid (1 ml.), water (4 ml.), methanol (20 ml.) and tetrahydrofuran (30 ml.) was subjected to catalytic reduction at room temperature under ordinary pressure for 6 hours. After removing the insoluble substance from the resultant mixture by filtration, the filtrate was concentrated in vacuo. Water was added to the residue and adjusted to pH 7 to 8 with sodium bicarbonate, and the insoluble substance was filtered out. The filtrate was washed with ethyl acetate and adjusted to pH 3.0 with conc. hydrochloric acid under ice cooling. The precipitates were collected by filtration, washed with water and dried over phosphorus pentoxide to give 7-[2-(2-aminothiazol-4-yl)-2-benzyloxyiminoacetamido]-3-cephem-4-carboxylic acid (syn isomer, 1.1 g.).

WORKUP

后处理

  1. customAfter removing the insoluble substance from the resultant mixture
  2. filtrationby filtration
  3. concentrationthe filtrate was concentrated in vacuo
  4. additionWater was added to the residue
  5. filtrationthe insoluble substance was filtered out
  6. washThe filtrate was washed with ethyl acetate
  7. filtrationThe precipitates were collected by filtration
  8. washwashed with water
  9. dry with materialdried over phosphorus pentoxide