تفاعل #1553567

معادلة التفاعل

N-methylhydrazine

Ethyl 4,4-difluoroacetoacetate

→

3-(difluoromethyl)-1-methyl-1H-pyrazol-5(4H)-one

المذيبات

toluene

toluene

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction mixture evaporated to dryness
2. 2
   أخرىThe resulting material was triturated with methyl t-butylether/heptane

الإجراء التجريبي

Ethyl 4,4-difluoroacetoacetate (30.12 g, 0.172 mol) was stirred in toluene (600 mL) over ice water. Solution of N-methylhydrazine (7.6 mL, 0.14 mol) in toluene (200 mL) was added slowly, dropwise over 20 min. The reaction mixture was heated at 100° C. for 2 hours. The reaction mixture evaporated to dryness. The resulting material was triturated with methyl t-butylether/heptane to give 3-(difluoromethyl)-1-methyl-1H-pyrazol-5(4H)-one in three batches (total 10.7 g, 51%) as orange powder. This material was used without further purification for the next reaction.

المصدر