HRID1658821

反应详情

EQUATION

反应方程式

HRID 1658821 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customInitially, a thick slurry resulted
  2. temperatureThe mixture was then heated
  3. temperatureat reflux for approximately two hours
  4. temperatureafter cooling to 25°C
  5. filtrationwas filtered
  6. washThe collected solid was washed with fresh methanol
  7. customdried in vacuo at 50°C