HRID1032542

反应详情

EQUATION

反应方程式

HRID 1032542 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

At 0° C., 1.2 g of N,N-dimethyl-N-[2-(7-amino-1H-indazol-4-yl)ethyl]amine in 10 ml of dimethylformamide and 5 ml of tetrahydrofuran is combined with 0.91 ml of methanesulfonyl chloride The mixture is agitated for 2 hours at 0° C. and for 14 hours at room temperature. The product is chromatographed on silica gel with methanol/dichloromethane 1:1 and treated with ethereal hydrochloric acid, obtaining, after recrystallization from methanol/diethyl ether, 550 mg of N-[4-(2-dimethylamino-ethyl)-1H-indazol-7-yl]methanesulfonamide, hydrochloride, mp 203°-205° C.

WORKUP

后处理

  1. customAt 0° C.
  2. customThe product is chromatographed on silica gel with methanol/dichloromethane 1:1
  3. additiontreated with ethereal hydrochloric acid
  4. customobtaining
  5. customafter recrystallization from methanol/diethyl ether, 550 mg of N-[4-(2-dimethylamino-ethyl)-1H-indazol-7-yl]methanesulfonamide, hydrochloride, mp 203°-205° C.