Hydrochloric Acid → 3-(Difluoromethyl)-1-methyl-4,5-dihydro-1H-pyrazole-4-carboxylic acid

HRID 1674486ノート

反応式

HRID 1674486 の反応式
C([O:3][C:4]([CH:6]1[CH2:10][N:9]([CH3:11])[N:8]=[C:7]1[CH:12]([F:14])[F:13])=[O:5])C.[OH-].[Na+].Cl>O1CCOCC1>[F:14][CH:12]([F:13])[C:7]1[CH:6]([C:4]([OH:5])=[O:3])[CH2:10][N:9]([CH3:11])[N:8]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67338397HCID 67338397、化合物

生成物 1

HCID 673384023-(Difluoromethyl)-1-methyl-4,5-dihydro-1H-pyrazole-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

3-Difluoromethyl-1-methyl-4,5-dihydro-1H-pyrazole-4-carboxylic acid ethyl ester (0.15 g, 0.7 mmol) was dissolved in 2 ml of dioxan. 1.5 ml of a 1 N aqueous sodium hydroxide solution (1.5 mmol) were added and the reaction mixture was stirred for 2 h at room temperature. Subsequently the mixture was acidified with concentrated hydrochloric acid (pH 2). The dioxan was removed in vacuo, the residue was extracted with ethyl acetate. The combined organic layer was washed with brine, dried over magnesium sulfate and evaporated, delivering 0.1 g of 3-difluoromethyl-1-methyl-4,5-dihydro-1H-pyrazole-4-carboxylic acid, which could be directly used in the next step without further purification.

後処理

  1. customThe dioxan was removed in vacuo
  2. extractionthe residue was extracted with ethyl acetate
  3. washThe combined organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customcould be directly used in the next step without further purification

出典と根拠

ORDレコード
ord-023bbf28d75a4b4eb829840f5435e97c
出典データセット
uspto-grants-2011_08
特許番号
US08003626B2

反応ノート

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