Water → (5-Chloro-3-(difluoromethyl)-1-methyl-1H-pyrazol-4-yl)methanol

HRID 1172116노트

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HRID 1172116 반응식
[Cl:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([CH:8]([F:10])[F:9])[C:3]=1[CH:11]=[O:12].[BH4-].[Na+].O>CO>[Cl:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([CH:8]([F:9])[F:10])[C:3]=1[CH2:11][OH:12]

참가 물질

5

반응물 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 197546925-Chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbaldehyde

생성물 1

HCID 17862871(5-Chloro-3-(difluoromethyl)-1-methyl-1H-pyrazol-4-yl)methanol수율 52.2%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

A solution of 7.2 g (37.0 mmoles) of 5-chloro-3-difluoromethyl-1-methyl-1H-pyrazole-4-carboaldehyde dissolved in 100 ml of methanol was cooled to 0° C. Thereto was gradually added 2.1 g (55.5 mmoles) of sodium borohydride. The mixture was stirred at room temperature for 3 hours to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The resulting organic layer was washed with an aqueous sodium chloride solution and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to vacuum distillation to remove the solvent contained therein, to obtain 3.8 g (yield: 52.1%) of (5-chloro-3-difluoromethyl-1-methyl-1H-pyrazol-4-yl)-methanol.

후처리

  1. customto give rise
  2. customto a reaction
  3. customAfter the completion of the reaction
  4. extractionfollowed by extraction with ethyl acetate
  5. washThe resulting organic layer was washed with an aqueous sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe resulting solution was subjected to vacuum distillation
  8. customto remove the solvent

출처 및 근거

ORD 기록
ord-3379d62eda454256ba139fd832e9888b
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07833939B2

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