HRID242086

反应详情

EQUATION

反应方程式

HRID 242086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

The crude 1-[1-(4-chlorophenyl)cyclobutyl]-7-methoxy-3,4-dihydroisoquinoline (10.25 g, 30.8 mmol) was treated with 47% aqueous hydrobromic acid (109 mL) and stirred at 120° C. for 4 h. The reaction mixture was cooled to room temperature. The aqueous layer was decanted. The crude product was treated with dichloromethan, methanol and water and the pH was adjusted to 10 with aqueous 1N sodium hydroxide solution. The product precipitated and the solid was collected by filtration. The product was washed with water and dried in vacuo at 30° C. Yield: 3.56 g (30.3, 12.38 mmol).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customThe aqueous layer was decanted
  3. additionThe crude product was treated with dichloromethan, methanol and water
  4. customThe product precipitated
  5. filtrationthe solid was collected by filtration
  6. washThe product was washed with water
  7. customdried in vacuo at 30° C