Chlorodifluoromethane → HCID 11357876, 화합물

HRID 2182809노트

반응식

HRID 2182809 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:12]=[C:11]([OH:13])[N:10]([CH3:14])[N:9]=2)=[C:4]([F:15])[CH:3]=1.[OH-].[Na+].Cl[CH:19]([F:21])[F:20]>O1CCOCC1.O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:12]=[C:11]([O:13][CH:19]([F:21])[F:20])[N:10]([CH3:14])[N:9]=2)=[C:4]([F:15])[CH:3]=1

참가 물질

6

반응물 3

HCID 6372ChlorodifluoromethaneHCID 14798Sodium HydroxideHCID 178481736HCID 178481736, 화합물

생성물 1

HCID 11357876HCID 11357876, 화합물수율 82.6%

시약·촉매·용매 2

HCID 962Water용매2회HCID 312751,4-Dioxane용매

실험 절차

57.1 g of 3-(4-chloro-2-fluorophenyl)-5-hydroxy-1-methyl-1H-pyrazole from Example 2.1 were initially charged in 500 ml of dioxane. A solution of 18.8 g of NaOH in 50 ml of H2O was added, the mixture was heated at reflux and 85 g (0.98 mol=3.9 eq.) of gaseous chlorodifluoromethane were introduced. The mixture was poured into 1.5 l of water and extracted twice with 500 ml of MTBE, and the combined organic phases were extracted once with 500 ml of water and once with 500 ml of saturated sodium chloride solution. Drying and concentration of the organic phase gave 57.6 g of 53% pure 3-(4-chloro-2-fluorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole as an oil which was purified further by vacuum distillation. This gave the title compound in a purity of 94% in a yield of 43.8%.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux
  3. extractionextracted twice with 500 ml of MTBE
  4. extractionthe combined organic phases were extracted once with 500 ml of water and once with 500 ml of saturated sodium chloride solution
  5. customDrying

출처 및 근거

ORD 기록
ord-fa01c0f2003140dd8048afef86c570cf
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06897322B2

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