HRID1658821
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 2 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