HRID67967

反应详情

EQUATION

反应方程式

HRID 67967 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trans-1,2-diamino-7-bromo-1,2,3,4-tetrahydronaphthalene (6.75 g, 28.0 m mol) was dissolved in ethanol (70 ml) and carbon disulfide (1.9 ml, 31.7 m mol) was added to the solution. After stirring at room temperature for 20 minutes, they were heated under reflux for 5.5 hours. The reaction mixture was cooled in an ice bath and crystals precipitated were collected by filtration, whereby trans-8-bromo-3a,4,5,9b-tetrahydronaphth[1,2-d]imidazoline-2-thione (5.57 g) was obtained in 70% yield. The crystals were recrystallized from methanol-acetonitrile to give pale-yellow crystals melting at 259.5°-260.5° C. (decomposition). The product gave the following data on spectroscopy and elemental analysis.

WORKUP

后处理

  1. temperaturethey were heated
  2. temperatureunder reflux for 5.5 hours
  3. temperatureThe reaction mixture was cooled in an ice bath
  4. customcrystals precipitated
  5. filtrationwere collected by filtration