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

HRID 2182814ノート

反応式

HRID 2182814 の反応式
[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

参加物

6

反応物 4

HCID 962WaterHCID 6372ChlorodifluoromethaneHCID 11430Potassium CarbonateHCID 178481735HCID 178481735、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c8355fcfd6ab4689a919a179a6e43e1a
出典データセット
uspto-grants-2005_05
特許番号
US06897322B2

反応ノート

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