反应 #1365750

反应方程式

4-t-Butyl-3-chloro-6-hydrazinopyridazine

dichloroacetic acid

→

solid

收率 74.0%

7-t-Butyl-6-chloro-3-dichloromethyl-1,2,4-triazolo[4,3-b]pyridazine

收率 74.0%

溶剂

toluene

反应条件

后处理

1. 1
   其他The toluene was removed
2. 2
   workup.ADDITIONthe residue was poured into water
3. 3
   其他to precipitate the product as a brown solid
4. 4
   其他The product was purified by chromotography on silica gel using 10% ethyl acetate/dichloromethane as eluant

实验过程

4-t-Butyl-3-chloro-6-hydrazinopyridazine (9.5 g, 48 mmol) and dichloroacetic acid (20 ml) were heated in toluene (130 ml) under Dean Stark conditions for 2.5 hours. The toluene was removed and the residue was poured into water to precipitate the product as a brown solid. The product was purified by chromotography on silica gel using 10% ethyl acetate/dichloromethane as eluant to yield a yellow solid (10.4 g, 74%), 1H NMR (250 MHz, CDCl3) δ 1.59 (9H, s, t-Bu), 6.01 (1H, s, CH), 8.37 (1H, s, ArH); MS (ES+) m/e 293 [MH]+.

来源