HRID387658

反应详情

EQUATION

反应方程式

HRID 387658 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.36 g of methyl[2-(2-bromophenyl)ethyl]carbamate and 5.2 g of phosphoric acid are stirred under an inert atmosphere at a temperature close to 150° C. The reaction mixture is cooled to a temperature close to 20° C., then it is hydrolysed with a mixture of water and ethyl acetate using ultrasound treatment. After decanting, the organic phase is washed with a saturated aqueous solution of sodium hydrogen carbonate, water, a saturated aqueous solution of sodium chloride, then concentrated using a rotary evaporator under reduced pressure (5 kPa). 0.105 g of 5-bromo-3,4-dihydroisoquinolin-1(2H)-one is obtained in the form of an amorphous beige solid.

WORKUP

后处理

  1. customclose to 150° C
  2. temperatureThe reaction mixture is cooled to a temperature
  3. customclose to 20° C.
  4. customAfter decanting
  5. washthe organic phase is washed with a saturated aqueous solution of sodium hydrogen carbonate, water
  6. concentrationa saturated aqueous solution of sodium chloride, then concentrated
  7. customa rotary evaporator under reduced pressure (5 kPa)