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Dimethylcarbamoyl Chloride → 3,5-Dimethyl-2-[4-[4-(N,N-dimethylcarbamoyloxy)-benzoyl]benzylthio]-4(3H)-quinazolinone

HRID 1291372
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HRID 1291372 반응식
[OH:1][C:2]1[CH:30]=[CH:29][C:5]([C:6]([C:8]2[CH:28]=[CH:27][C:11]([CH2:12][S:13][C:14]3[N:23]([CH3:24])[C:22](=[O:25])[C:21]4[C:16](=[CH:17][CH:18]=[CH:19][C:20]=4[CH3:26])[N:15]=3)=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.[CH3:31][N:32]([CH3:36])[C:33](Cl)=[O:34].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:24][N:23]1[C:22](=[O:25])[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][C:20]=2[CH3:26])[N:15]=[C:14]1[S:13][CH2:12][C:11]1[CH:27]=[CH:28][C:8]([C:6](=[O:7])[C:5]2[CH:4]=[CH:3][C:2]([O:1][C:33](=[O:34])[N:32]([CH3:36])[CH3:31])=[CH:30][CH:29]=2)=[CH:9][CH:10]=1
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참가 물질

5

반응물 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 11430Potassium CarbonateHCID 189188882-[4-(4-hydroxybenzoyl)benzylthio]-3,5-dimethyl-4(3H)-quinazolinone

생성물 1

HCID 189190183,5-Dimethyl-2-[4-[4-(N,N-dimethylcarbamoyloxy)-benzoyl]benzylthio]-4(3H)-quinazolinone

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 2-[4-(4-hydroxybenzoyl)benzylthio]-3,5-dimethyl-4(3H)-quinazolinone (478 mg), dimethylcarbamoyl chloride (0.15 ml) and potassium carbonate (315 mg) in DMF (7 ml) was stirred at 50° C. for 48 hours. This reaction mixture was concentrated and the residue was dissolved in ethyl acetate. The solution was washed with water, dried, and concentrated. The residue was recrystallized from ethyl acetate to provide the title compound as colorless solid (346 mg).

후처리

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe solution was washed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-03d71a37215f44438f68b05d0cd266a2
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753664

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