HRID1036640

反应详情

EQUATION

反应方程式

HRID 1036640 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of hydroxylamine-O-sulfonic acid (2) (2 g, 1 equiv), water (10 mL) and isoquinoline (1) (6.3 mL, 3 equiv) was heated at 90° C. for 2-3 h. Potassium carbonate (2.44 g, 1 equiv) was added, and the water was evaporated. Ethanol (20-30 mL) was added to the solid residue, and insoluble potassium sulfate was filtered out. Hydroiodic acid (57%-67%, 1.34 mL, 1 equiv) was added to the filtrate, and the resulting solution was placed in a freezer. The precipitate was filtered out, washed with ethanol, and dried in vacuo. Isolated products were used as such in further reactions. Yield of the product was 1.78 g.

WORKUP

后处理

  1. customthe water was evaporated
  2. additionEthanol (20-30 mL) was added to the solid residue, and insoluble potassium sulfate
  3. filtrationwas filtered out
  4. filtrationThe precipitate was filtered out
  5. washwashed with ethanol
  6. customdried in vacuo