反応 #63230

反応方程式

tetra-n-butylammonium hydroxide

sodium hydroxide

4-chloro-1-hydroxypyrazole

chloromethyl thiocyanate

→

4-chloro-1-[(thiocyanato)-methoxy]-pyrazole

収率 71.6%

溶媒

methylene chloride

反応条件

後処理

1. 1
   その他Thereafter, the organic phase was separated off
2. 2
   その他dried
3. 3
   その他evaporated down
4. 4
   workup.DISTILLATIONDistillation of the residue under reduced pressure (airbath at 140° C./3 mbar)

実験手順

50 ml of a 5% strength aqueous sodium hydroxide solution were added to 5 g (42 mMol) of 4-chloro-1-hydroxypyrazole, 13.5 g (126 mMol) of chloromethyl thiocyanate and 50 ml of methylene chloride. After the addition of 1 g (4 mMol) of tetra-n-butylammonium hydroxide, the mixture was stirred at room temperature for 24 hours. Thereafter, the organic phase was separated off, dried and evaporated down. Distillation of the residue under reduced pressure (airbath at 140° C./3 mbar) gave 5.7 g (71% of theory) of 4-chloro-1-[(thiocyanato)-methoxy]-pyrazole (compound No. 1), which was recrystallized from ether/petroleum ether (mp. 60° C.).

出典