Methanol → N-[6-(4-Hydroxycyclohex-1-en-1-yl)-5-methylpyridin-3-yl]-5-methyl-1-[4-(trifluoromethyl)-phenyl]-1H-pyrazole-4-carboxamide

HRID 1748647ノート

反応式

HRID 1748647 の反応式
[BH4-].[Na+].[CH3:3][C:4]1[CH:5]=[C:6]([NH:17][C:18]([C:20]2[CH:21]=[N:22][N:23]([C:25]3[CH:30]=[CH:29][C:28]([C:31]([F:34])([F:33])[F:32])=[CH:27][CH:26]=3)[CH:24]=2)=[O:19])[CH:7]=[N:8][C:9]=1[C:10]1[CH2:15][CH2:14][C:13](=[O:16])[CH2:12][CH:11]=1.[OH-].[Na+].[CH3:37]O>>[OH:16][CH:13]1[CH2:14][CH2:15][C:10]([C:9]2[N:8]=[CH:7][C:6]([NH:17][C:18]([C:20]3[CH:21]=[N:22][N:23]([C:25]4[CH:26]=[CH:27][C:28]([C:31]([F:34])([F:32])[F:33])=[CH:29][CH:30]=4)[C:24]=3[CH3:37])=[O:19])=[CH:5][C:4]=2[CH3:3])=[CH:11][CH2:12]1

参加物

5

反応物 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 86692586N-[5-methyl-6-(4-oxocyclohex-1-en-1-yl)pyridin-3-yl]-1-[4-(trifluoromethyl)phenyl]-1H-pyrazole-4-carboxamide

生成物 1

HCID 86692587N-[6-(4-Hydroxycyclohex-1-en-1-yl)-5-methylpyridin-3-yl]-5-methyl-1-[4-(trifluoromethyl)-phenyl]-1H-pyrazole-4-carboxamide

実験手順

Sodium borohydride (19 mg) was added to a solution of N-[5-methyl-6-(4-oxocyclohex-1-en-1-yl)pyridin-3-yl]-1-[4-(trifluoromethyl)phenyl]-1H-pyrazole-4-carboxamide (114 mg) in methanol (15 ml) under ice-cooling and the mixture was stirred at the same temperature for 30 minutes. After the reaction, 1N aqueous solution of sodium hydroxide was added and the organic solvent was evaporated. The precipitated solid was washed with water, filtered and dried at 60° C. under current of air to give the titled compound (110 mg) as a white solid.

後処理

  1. temperaturecooling
  2. additionwas added
  3. customthe organic solvent was evaporated
  4. washThe precipitated solid was washed with water
  5. filtrationfiltered
  6. customdried at 60° C. under current of air

出典と根拠

ORDレコード
ord-96899710458242b6a27b7b48bbebeaad
出典データセット
uspto-grants-2015_10
特許番号
US09150555B2

反応ノート

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