HRID902996

反应详情

EQUATION

反应方程式

HRID 902996 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 14.2 grams (0.2 mole) pyrrolidine in 100 milliliters ether was added 23.8 grams (0.1 mole) 3-trichloromethyl-5-chloro-1,2,4-thiadiazole in 100 milliliters ether. The solution was refluxed with stirring for one hour after addition. Filtration to remove salt by-products yielded a clear filtrate which was concentrated on a steam bath to give 16.4 grams (60% molar yield) of white solid. Recrystallization from ligroin yielded a pure product (melting point 105.5°-107° C.). The structure was confirmed via infrared and elemental analysis. Analysis for C7H8N3Cl3S:

WORKUP

后处理

  1. temperatureThe solution was refluxed
  2. additionafter addition
  3. filtrationFiltration
  4. customto remove salt by-products
  5. customyielded a clear filtrate which
  6. concentrationwas concentrated on a steam bath
  7. customto give
  8. custom16.4 grams (60% molar yield) of white solid
  9. customRecrystallization from ligroin