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Dimethylformamide → (2E)-3-(dimethylamino)-1-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]prop-2-en-1-one

HRID 1843661
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HRID 1843661 반응식
[CH3:1][O:2][C:3]1[CH:26]=[CH:25][C:6]([CH2:7][N:8]2[CH:12]=[C:11]([C:13](=[O:15])[CH3:14])[C:10]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([N+:22]([O-:24])=[O:23])[CH:17]=3)=[N:9]2)=[CH:5][CH:4]=1.[CH3:27][N:28]([CH3:31])[CH:29]=O>O1CCCC1>[CH3:27][N:28]([CH3:31])/[CH:29]=[CH:14]/[C:13]([C:11]1[C:10]([C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([N+:22]([O-:24])=[O:23])[CH:17]=2)=[N:9][N:8]([CH2:7][C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:26][CH:25]=2)[CH:12]=1)=[O:15]
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참가 물질

4

반응물 2

HCID 6228DimethylformamideHCID 67185282HCID 67185282, 화합물

생성물 1

HCID 67186714(2E)-3-(dimethylamino)-1-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]prop-2-en-1-one수율 96%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
70 °C

실험 절차

460 mg (1.3 mmol) of 1-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]-ethanone were dissolved in 25 ml of dry tetrahydrofuran and 15 ml of dimethylformamide di-tert-butylacetale (62 mmol) were added to the resulting solution. The reaction was heated at 70° C. under stirring for 6 hours. The solvent was then evaporated in vacuo and the residue diluted with dichloromethane and washed with water. The organic layer was finally dried over sodium sulphate and evaporated, giving 500 mg (96%) of the title compound as an oil.

후처리

  1. customThe solvent was then evaporated in vacuo
  2. additionthe residue diluted with dichloromethane
  3. washwashed with water
  4. dry with materialThe organic layer was finally dried over sodium sulphate
  5. customevaporated

출처 및 근거

ORD 기록
ord-1e3c8fcaf1ea4272bf270592f133e621
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946250B2

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