Dimethylformamide → 2-[4-(4-Chlorobenzoyl)benzyl]thio-3,5-dimethylthieno[2,3-d]pyrimidin-4(3H)-one

HRID 1291331노트

반응식

HRID 1291331 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+].CN(C=O)C.[Cl:21][C:22]1[CH:37]=[CH:36][C:25]([C:26]([C:28]2[CH:35]=[CH:34][C:31]([CH2:32]Br)=[CH:30][CH:29]=2)=[O:27])=[CH:24][CH:23]=1>CO.O>[Cl:21][C:22]1[CH:23]=[CH:24][C:25]([C:26]([C:28]2[CH:35]=[CH:34][C:31]([CH2:32][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:30][CH:29]=2)=[O:27])=[CH:36][CH:37]=1

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 14798Sodium HydroxideHCID 98396514-(4-Chlorobenzoyl)benzyl bromideHCID 178431876HCID 178431876, 화합물

생성물 1

HCID 189191282-[4-(4-Chlorobenzoyl)benzyl]thio-3,5-dimethylthieno[2,3-d]pyrimidin-4(3H)-one수율 39.9%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

To a solution of 3,5-dimethyl-2-mercaptothieno[2,3-d]pyrimidin-4(3H)-one (1.06 g) and sodium hydroxide (205 mg) in 50% methanol (16 ml)-DMF (4 ml) was added 4-(4-chlorobenzoyl)benzyl bromide (1.69 g) and the mixture was stirred at room temperature for 1 hour. This reaction mixture was poured in water and the resulting crystals were collected by filtration, rinsed with water, and recrystallized from ethyl acetate to provide the title compound as colorless solid (878 mg).

후처리

  1. filtrationthe resulting crystals were collected by filtration
  2. washrinsed with water
  3. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-1a2e708edc094e94b18bee23c363da57
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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