HRID660904
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
A solution of 3.41 g (12.27 mmol) of the compound from Example 231A in 14 ml methanol/water (7:3) is added dropwise to a solution of 995 mg (12.27 mmol) of potassium isocyanate in 11 ml methanol/water (7:3). This is stirred for 1 hr at RT. The thick suspension is diluted with 7.4 ml water and 39 ml methanol to facilitate stirring, then heated under reflux for 1 hr and then left to stand overnight at RT. After cooling to 0° C., the precipitate is filtered off, washed with ice-cold water and dried overnight in the drying cabinet at 60° C. 2.84 g (76% of theory) of the title compound are obtained.
WORKUP
后处理
- stirringto facilitate stirring
- temperatureheated
- temperatureunder reflux for 1 hr
- waitleft
- waitto stand overnight at RT
- temperatureAfter cooling to 0° C.
- filtrationthe precipitate is filtered off
- washwashed with ice-cold water
- customdried overnight in the drying cabinet at 60° C