HRID2289805
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
LRMS 180, 182 (MH+), 359, 361, 363 (M2H+). ##STR108## 4-Chloro-1-(2H)-isoquinolone (20.62 g, 115 mmol) was added portionwise to stirred chlorosulphonic acid (61 mL, 918 mmol) at 0° C. The mixture was heated at 100° C. for 3.5 d and then cooled to room temperature. The reaction mixture was added in small portions onto ice-water [CAUTION] and the resulting precipitate was collected by filtration. The solid was washed with water, triturated with MeCN and then dried in vacuo to give 4-chloro-1-oxo-1,2-dihydro-7-isoquinolinesulphonyl chloride (18.75 g, 67.4 mmol) as a cream solid.
WORKUP
后处理
- temperaturecooled to room temperature
- additionThe reaction mixture was added in small portions onto ice-water [CAUTION]
- filtrationthe resulting precipitate was collected by filtration
- washThe solid was washed with water
- customtriturated with MeCN
- customdried in vacuo