HRID2351144

反应详情

EQUATION

反应方程式

HRID 2351144 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of benzhydryl 7-formamido-3 -[(Z)-2-(3-pyridyl)vinylthio]-3-cephem-4-carboxylate (69.8 g) in methanol (350 ml) was added conc. hydrochloric acid (40.7 ml). The mixture was heated at 30°-35° C. for 2 hours. The mixture was poured into a mixture of ethyl acetate (2 l) and water (1 l) and adjusted to pH 6.5 with a saturated aqueous solution of sodium bicarbonate. The organic layer was separated, washed with water and saturated aqueous solution of sodium chloride in turn, dried over magnesium sulfate and concentrated in vacuo to a crystal. The crystal was washed with diethyl ether to give benzhydryl 7-amino-3-[(Z)-2-(3-pyridyl)vinylthio]-3-cephem-4-carboxylate (52.3 g).

WORKUP

后处理

  1. temperatureThe mixture was heated at 30°-35° C. for 2 hours
  2. customThe organic layer was separated
  3. washwashed with water and saturated aqueous solution of sodium chloride in turn
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo to a crystal
  6. washThe crystal was washed with diethyl ether