Water → Methyl 5-(difluoromethoxy)-1-methyl-1H-pyrazole-3-carboxylate

HRID 362651

반응식

HRID 362651 반응식
[OH:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([O:10][CH3:11])=[O:9])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH:19]([F:21])[F:20].O>CN(C)C=O>[F:20][CH:19]([F:21])[O:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([O:10][CH3:11])=[O:9])[CH:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6372ChlorodifluoromethaneHCID 11430Potassium CarbonateHCID 178498595HCID 178498595, 화합물

생성물 1

HCID 54319416Methyl 5-(difluoromethoxy)-1-methyl-1H-pyrazole-3-carboxylate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

67.6 g (0.43 mol) 5-Hydroxy-3-methoxycarbonyl-1-methylpyrazole and 299.2 g (2.17 mol) potassium carbonate was dissolved in 1500 ml dimethylformamide and heated to 70° C. At this temperature chlorodifluoromethane was introduced over 2 hours and the mixture stirred at 80° C. for 1.5 hours. The reaction mixture was added to water and extracted 6 times with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The reaction solution was concentrated.

후처리

  1. extractionextracted 6 times with ethyl acetate
  2. washThe combined organic phases were washed with saturated aqueous sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. concentrationThe reaction solution was concentrated

출처 및 근거

ORD 기록
ord-00d102e2297d4b64bd63ab720ce4305c
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05869686

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