반응 #63230

반응 방정식

tetra-n-butylammonium hydroxide

sodium hydroxide

4-chloro-1-hydroxypyrazole

chloromethyl thiocyanate

→

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

수율 71.6%

용매

methylene chloride

반응 조건

후처리

1. 1
   기타Thereafter, the organic phase was separated off
2. 2
   기타dried
3. 3
   기타evaporated down
4. 4
   workup.DISTILLATIONDistillation of the residue under reduced pressure (airbath at 140° C./3 mbar)

실험 절차

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.).

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