Dimethylformamide → 2-[4-(4-Acetoxybenzoyl)benzylthio]-3,5-dimethylthieno[2,3-d]pyrimidin-4(3H)-one

HRID 1291339노트

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HRID 1291339 반응식
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[C:9]([CH3:12])=[CH:10][S:11][C:5]=2[N:4]=[C:3]1[SH:13].[OH-].[Na+].O.CN(C=O)C.[C:22]([O:25][C:26]1[CH:41]=[CH:40][C:29]([C:30]([C:32]2[CH:39]=[CH:38][C:35]([CH2:36]Br)=[CH:34][CH:33]=2)=[O:31])=[CH:28][CH:27]=1)(=[O:24])[CH3:23]>C(O)C.O>[C:22]([O:25][C:26]1[CH:41]=[CH:40][C:29]([C:30]([C:32]2[CH:33]=[CH:34][C:35]([CH2:36][S:13][C:3]3[N:2]([CH3:1])[C:7](=[O:8])[C:6]4[C:9]([CH3:12])=[CH:10][S:11][C:5]=4[N:4]=3)=[CH:38][CH:39]=2)=[O:31])=[CH:28][CH:27]=1)(=[O:24])[CH3:23]

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 189192074-(4-Acetoxybenzoyl)benzyl bromideHCID 23719242Sodium hydroxide--water (1/1/1)HCID 178431876HCID 178431876, 화합물

생성물 1

HCID 189192392-[4-(4-Acetoxybenzoyl)benzylthio]-3,5-dimethylthieno[2,3-d]pyrimidin-4(3H)-one수율 29%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

To a solution of 3,5-dimethyl-2-mercaptothieno[2,3-d]pyrimidin-4(3H)-one (1.40 g) and 1N-sodium hydroxide/water (6.7 ml) in ethanol (13 ml)-DMF (25 ml) was added 4-(4-acetoxybenzoyl)benzyl bromide (2.68 g) and the mixture was stirred at room temperature at 60° C. for 1 hour. This reaction mixture was poured in water and extracted with ethyl acetate. The extract was washed with water, dried, and concentrated, and the residue was recrystallized from methanol to provide the title compound as colorless solid (887 mg).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. concentrationconcentrated
  5. customthe residue was recrystallized from methanol

출처 및 근거

ORD 기록
ord-ef82eec2593b49b6b179ab00753fd34a
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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