HRID436858
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
To a stirred solution of 49.7 parts of 2-oxo-4-thioxothiazolidine in 990 parts of methanol there was added at 40° C. and under an atmosphere of nitrogen 54.3 parts of powdered 1,3-diiminoisoindoline. Initially, a thick slurry resulted. The reaction mixture was stirred at room temperature for two hours during which time the mixture gradually thinned. The mixture was then heated at reflux for approximately two hours and after cooling to 25° C., was filtered. The collected solid was washed with fresh methanol and dried in vacuo at 50° C. to obtain 1-imino-3-(2-oxo-4-thioxo-5-thiazolidinylidene)isoindoline as an orange powder melting at 267°-8° C. (dec.).
WORKUP
后处理
- customInitially, a thick slurry resulted
- temperatureThe mixture was then heated
- temperatureat reflux for approximately two hours
- temperatureafter cooling to 25° C.
- filtrationwas filtered
- washThe collected solid was washed with fresh methanol
- customdried in vacuo at 50° C.