反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The remainder of the solution of the 2-bromo-3-bromomethyl compound obtained was used as such in the following debromination process. To this solution which contained at most 14.4 mmoles of t-butyl 7-benzamido-2-bromo-3-bromomethyl-3-cephem-4-carboxylate 1-oxide, were added 14 ml (approximately 25 mmoles) of triisodecyl phosphite and the mixture was stirred for 30 minutes at room temperature. The reaction mixture was then washed with water, dried over magnesium sulfate and filtered. The filtrate was evaporated to dryness and upon addition of a small quantity of acetone, a brown precipitate was formed. Upon addition of diethyl ether, the brown precipitate was decolored almost completely and after standing for one night in the refrigerator, the precipitate was filtered off to obtain 3.0 g (44.6%) of t-butyl 7-benzamido-3-bromomethyl-3-cephem-4-carboxylate 1-oxide.
WORKUP
后处理
- washThe reaction mixture was then washed with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customThe filtrate was evaporated to dryness and upon addition of a small quantity of acetone
- customa brown precipitate was formed
- waitafter standing for one night in the refrigerator
- filtrationthe precipitate was filtered off