Water → (5-chloro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol

HRID 1172094ノート

反応式

HRID 1172094 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[N:12]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:11]=[C:10]([C:19]([F:22])([F:21])[F:20])[C:9]=1[CH:23]=[O:24].C(OCC)(=O)C.O>C1COCC1>[Cl:7][C:8]1[N:12]([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[N:11]=[C:10]([C:19]([F:21])([F:20])[F:22])[C:9]=1[CH2:23][OH:24]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 14790525-chloro-1-phenyl-3-(trifluoromethyl)-1H-pyrazole-4-carbaldehydeHCID 21226445Aluminium lithium hydride

生成物 1

HCID 17862912(5-chloro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol収率 99.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-30 °C

実験手順

A solution of 0.21 g (5.5 mmoles) of lithium aluminum hydride dissolved in 70 ml of THF was cooled to −30° C. Thereto was gradually added a solution of 3 g (10.9 mmoles) of 5-chloro-1-phenyl-3-trifluoromethyl-1H-pyrazole-4-carboaldehyde dissolved in 30 ml of tetrahydrofuran. The resulting mixture was stirred at −30° C. for 30 minutes to give rise to a reaction. After the completion of the reaction, ethyl acetate was added, followed by stirring. Then, water was added, followed by stirring for a while. The reaction mixture was filtered under vacuum. The filtrate was extracted 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 3.0 g (yield: 99.9%) of (5-chloro-1-phenyl-3-trifluoromethyl-1H-pyrazol-4-yl)-methanol as white crystals.

後処理

  1. customto give rise
  2. customto a reaction
  3. additionwas added
  4. stirringby stirring
  5. stirringby stirring for a while
  6. filtrationThe reaction mixture was filtered under vacuum
  7. extractionThe filtrate was extracted with ethyl acetate
  8. washThe resulting organic layer was washed with an aqueous sodium chloride solution
  9. dry with materialdried over anhydrous magnesium sulfate
  10. distillationThe resulting solution was subjected to vacuum distillation
  11. customto remove the solvent

出典と根拠

ORDレコード
ord-11edac7a272d405db4a49225362489b9
出典データセット
uspto-grants-2010_11
特許番号
US07833939B2

反応ノート

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