HRID65034

反应详情

EQUATION

反应方程式

HRID 65034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 40 ml of acetonitrile was dissolved 1.12 g of benzyloxycarbonylaminothioacetamide. In the solution was suspended 2.0 g of 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide. To the suspension was added while stirring 0.8 ml of triethylamine. The mixture was stirred for 2 hours under reflux. The resultant was left standing for cooling, then the solvent was evaporated off. To the residue was added a saturated aqueous solution of sodium hydrogen carbonate. The mixture was subjected to extraction with ethyl acetate. The extract solution was washed with water, dried and, then, the solvent was evaporated off. The residue was recrystallized from ethyl acetate-isopropylether to give 1.3 g (yield 56%) of 2-(benzyloxycarbonylaminomethyl)-4-(4-methoxyphenyl)-5-(3-pyridyl)-1,3-thiazole, m.p. 93°-94° C.

WORKUP

后处理

  1. additionTo the suspension was added
  2. temperatureunder reflux
  3. waitThe resultant was left
  4. temperaturefor cooling
  5. customthe solvent was evaporated off
  6. additionTo the residue was added a saturated aqueous solution of sodium hydrogen carbonate
  7. extractionThe mixture was subjected to extraction with ethyl acetate
  8. washThe extract solution was washed with water
  9. customdried
  10. customthe solvent was evaporated off
  11. customThe residue was recrystallized from ethyl acetate-isopropylether