Dimethylformamide → HCID 23157275, 화합물

HRID 2110867노트

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HRID 2110867 반응식
[C:1]([C:5]1[CH2:6][C:7](=[O:10])[NH:8][N:9]=1)([CH3:4])([CH3:3])[CH3:2].Br[CH2:12][C:13]1[CH:22]=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][CH:14]=1.[C:23](=[O:26])([O-])[O-].[K+].[K+].CN(C)[CH:31]=[O:32]>O>[C:1]([C:5]1[CH:6]=[C:7]([O:10][CH2:12][C:13]2[CH:22]=[CH:21][C:16]([C:17]([O:19][CH3:20])=[O:18])=[CH:15][CH:14]=2)[N:8]([CH2:12][C:13]2[CH:22]=[CH:21][C:16]([C:23]([O:32][CH3:31])=[O:26])=[CH:15][CH:14]=2)[N:9]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 256687Methyl 4-(bromomethyl)benzoateHCID 5204213-tert-butyl-4,5-dihydro-1H-pyrazol-5-one

생성물 1

HCID 23157275HCID 23157275, 화합물수율 44%

시약·촉매·용매 1

HCID 962Water용매

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온도
60 °C

실험 절차

A mixture of 5-tert-butyl-2,4-dihydro-3H-pyrazol-3-one (5.00 g, 35.7 mmol), methyl 4-(bromomethyl)benzoate (17.16 g, 74.91 mmol), potassium carbonate (10.5 g, 76.0 mmol) and N,N-dimethylformamide (50 mL) was stirred overnight at 60° C. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract washed with aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography (ethyl acetate:hexane=1:3) to give the title compound (6.90 g, yield 44%) as a colorless oil. melting point 93-94° C.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract washed with aqueous sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8081945f9ee743c7bd1622db8e70da6c
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07517910B2

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