Hydrochloric Acid → 1-methyl-3-(pentafluoroethyl)-4-(trifluoromethyl)-1H-pyrazole-5-carboxylic acid

HRID 1843066노트

반응식

HRID 1843066 반응식
[C:1]([C:3]1[N:7]([CH3:8])[N:6]=[C:5]([C:9]([F:15])([F:14])[C:10]([F:13])([F:12])[F:11])[C:4]=1[C:16]([F:19])([F:18])[F:17])#N.[OH-:20].[Na+].Cl.[OH2:23]>>[CH3:8][N:7]1[C:3]([C:1]([OH:23])=[O:20])=[C:4]([C:16]([F:19])([F:18])[F:17])[C:5]([C:9]([F:15])([F:14])[C:10]([F:13])([F:12])[F:11])=[N:6]1

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 866600911-Methyl-3-(perfluoroethyl)-4-(trifluoromethyl)-1H-pyrazole-5-carbonitrile

생성물 1

HCID 866600921-methyl-3-(pentafluoroethyl)-4-(trifluoromethyl)-1H-pyrazole-5-carboxylic acid

반응 조건

온도
100 °C

실험 절차

11.0 g (37.5 mmol) of 5-cyano-1-methyl-3-pentafluoroethyl-4-trifluoromethyl-1H-pyrazole, 22 ml of 50% strength sodium hydroxide solution and 7.0 ml of distilled water are heated in an oil bath until the solid has dissolved. The reaction mixture is then stirred overnight (oil bath temperature 100° C.). After cooling, the reaction mixture is poured onto a mixture of 150 ml of concentrated hydrochloric acid and 150 ml of ice. The mixture is afterstirred for 30 minutes and the solid is filtered off. The solid is washed with a small amount of water and then dried in an oil pump vacuum. This gives 11.2 g (95%) of 1-methyl-3-pentafluoroethyl-4-trifluoromethyl-1H-pyrazole-5-carboxylic acid as a white solid.00

후처리

  1. dissolutionhas dissolved
  2. temperatureAfter cooling
  3. waitThe mixture is afterstirred for 30 minutes
  4. filtrationthe solid is filtered off
  5. washThe solid is washed with a small amount of water
  6. customdried in an oil pump vacuum

출처 및 근거

ORD 기록
ord-57585db7acf7416c927a88fbc3f82a95
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946234B2

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