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

HRID 1674486노트

반응식

HRID 1674486 반응식
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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67338397HCID 67338397, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-023bbf28d75a4b4eb829840f5435e97c
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003626B2

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