HRID839764

反应详情

EQUATION

反应方程式

HRID 839764 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of 6.0 g of 2-methylamino-5-(β-chloro-α,α-dimethylethyl)-1,3,4-thiadiazole in 100 ml of benzene was added 2.0 g of methyl isocyanate. The mixture became homogenous upon heating to reflux temperature and reflux was maintained for 2 hrs. After cooling, the benzene was removed at reduced pressure and the precipitate collected, giving 7.4 g (95%), m.p. 159°-161°. An analytical sample was prepared from methylene chloride-ether, m.p. 160°-161°.

WORKUP

后处理

  1. temperatureupon heating
  2. temperatureto reflux temperature
  3. temperaturereflux
  4. temperaturewas maintained for 2 hrs
  5. temperatureAfter cooling
  6. customthe benzene was removed at reduced pressure
  7. customthe precipitate collected
  8. customgiving 7.4 g (95%), m.p. 159°-161°