HRID21681

反应详情

EQUATION

反应方程式

HRID 21681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 50 ml of acetone were added 2.46 g of o-anisidine and 3.75 g of benzoyl isothiocyanate, and the mixture is stirred under reflux for 2 hours and, then, allowed to stand overnight in a refrigerator at 5° C. The resulting crystals were collected by filtration, washed with cold acetone and dried under reduced pressure. The crystals were added to 50 ml of 30% methylamine-methanol and the mixture was stirred at room temperature overnight. The reaction mixture was concentrated to dryness under reduced pressure, and the residue was washed with ethanol-ethyl acetate and dried under reduced pressure. The procedure provided 2.08 g of N-(o-methoxyphenyl)thiourea.

WORKUP

后处理

  1. temperatureunder reflux for 2 hours
  2. filtrationThe resulting crystals were collected by filtration
  3. washwashed with cold acetone
  4. customdried under reduced pressure
  5. additionThe crystals were added to 50 ml of 30% methylamine-methanol
  6. stirringthe mixture was stirred at room temperature overnight
  7. concentrationThe reaction mixture was concentrated to dryness under reduced pressure
  8. washthe residue was washed with ethanol-ethyl acetate
  9. customdried under reduced pressure