HRID615795

反应详情

EQUATION

反应方程式

HRID 615795 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of diphenylmethyl 7-[(Z)-2-methoxyimino-2-(2-tritylaminothiazol-4-yl)acetamido]-3-iodomethyl-3-cephem-4-carboxylate [VIIa] (237 mg, 0.29 mmole) and 2-(N-t-butoxycarbonylglycylamino)thiazolo[4,5-c]pyridine (95 mg, 0.31 mmole) in 2 ml of dry DMSO was allowed to stand at room temperature for 2 hours and then diluted with ether to give the crude quaternary salt, which was treated with 90% TFA and 2 drops of anisole at room temperature for 30 minutes. The mixture was evaporated and triturated with ether to afford 168 mg of pale yellow precipitate, which was purified by a column of HP-20 resin (40 ml) using 30% aqueous CH3OH as an eluant to give 88 mg of the title product Iq. Mp. 178°-187° C. (dec.). Estimated purity by HPLC: 60%.

WORKUP

后处理

  1. customto give the crude quaternary salt, which
  2. customThe mixture was evaporated
  3. customtriturated with ether