Water → 3-(2,4-Dichlorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole

HRID 2182814노트

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HRID 2182814 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:13]=[C:12]([OH:14])[N:11]([CH3:15])[N:10]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH:23]([F:25])[F:24].O>CC(N(C)C)=O>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:13]=[C:12]([O:14][CH:23]([F:25])[F:24])[N:11]([CH3:15])[N:10]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6372ChlorodifluoromethaneHCID 11430Potassium CarbonateHCID 178481735HCID 178481735, 화합물

생성물 1

HCID 156723613-(2,4-Dichlorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole수율 94%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

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온도
90 °C

실험 절차

9 g of 3-(2,4-dichlorophenyl)-5-hydroxy-1-methyl-1H-pyrazole from Example 4.1 were initially charged in 50 ml of dimethylacetamide, and 5.4 g of potassium carbonate were added. The mixture was heated at 90° C., and 48 g of gaseous chlorodifluoromethane were introduced over a period of 1 h. The mixture was poured into 800 ml of water and extracted twice with 300 ml of MTBE, and the combined organic phases were extracted once with 100 ml of water and once with 100 ml of saturated sodium chloride solution. Drying and concentration of the organic phase gave 10.2 g of 3-(2,4-dichlorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole of a purity of 56% (yield 50.2%, based on the title compound), which was purified further by vacuum distillation.

후처리

  1. extractionextracted twice with 300 ml of MTBE
  2. extractionthe combined organic phases were extracted once with 100 ml of water and once with 100 ml of saturated sodium chloride solution
  3. customDrying

출처 및 근거

ORD 기록
ord-c8355fcfd6ab4689a919a179a6e43e1a
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06897322B2

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