4-(4-Trifluoromethylbenzoyl)benzyl bromide → 3-Methyl-2-[4-(4-trifluoromethylbenzoyl) benzylthio]-thieno[3,2-d]pyrimidin-4(3H)-one

HRID 1291343노트

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HRID 1291343 반응식
[SH:1][C:2]1[N:3]([CH3:12])[C:4](=[O:11])[C:5]2[S:10][CH:9]=[CH:8][C:6]=2[N:7]=1.[F:13][C:14]([F:32])([F:31])[C:15]1[CH:30]=[CH:29][C:18]([C:19]([C:21]2[CH:28]=[CH:27][C:24]([CH2:25]Br)=[CH:23][CH:22]=2)=[O:20])=[CH:17][CH:16]=1>C(O)C.O.[OH-].[Na+].O>[CH3:12][N:3]1[C:4](=[O:11])[C:5]2[S:10][CH:9]=[CH:8][C:6]=2[N:7]=[C:2]1[S:1][CH2:25][C:24]1[CH:27]=[CH:28][C:21]([C:19](=[O:20])[C:18]2[CH:29]=[CH:30][C:15]([C:14]([F:13])([F:31])[F:32])=[CH:16][CH:17]=2)=[CH:22][CH:23]=1

참가 물질

6

반응물 2

HCID 189191184-(4-Trifluoromethylbenzoyl)benzyl bromideHCID 178481668HCID 178481668, 화합물

생성물 1

HCID 699607443-Methyl-2-[4-(4-trifluoromethylbenzoyl) benzylthio]-thieno[3,2-d]pyrimidin-4(3H)-one수율 47.8%

시약·촉매·용매 3

HCID 23719242Sodium hydroxide--water (1/1/1)촉매HCID 702Ethanol용매HCID 962Water용매

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온도
60 °C

실험 절차

To a solution of 2-mercapto-3-methylthieno[3,2-d]-pyrimidin-4(3H)-one (1.0 g) and 1N-sodium hydroxide/water (5.1 mg) in ethanol (10 ml) was added 4-(4-trifluoromethylbenzoyl)benzyl bromide (1.73 g) and the mixture was stirred at 60° C. 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-hexane to provide the title compound as colorless solid (1.11 g).

후처리

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

출처 및 근거

ORD 기록
ord-f1ac4dbedee2429ea2d46e2d03bcf98c
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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