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4-(2,4-Dichlorobenzoyl)benzyl bromide → 2-[4-(2,4-Dichlorobenzoyl)benzylthio]-3-methylthieno[3,2-d]pyrimidin-4(3H)-one

HRID 1291349
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HRID 1291349 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.[OH-].[Na+].O.[Cl:16][C:17]1[CH:32]=[C:31]([Cl:33])[CH:30]=[CH:29][C:18]=1[C:19]([C:21]1[CH:28]=[CH:27][C:24]([CH2:25]Br)=[CH:23][CH:22]=1)=[O:20]>C(O)C.O>[Cl:16][C:17]1[CH:32]=[C:31]([Cl:33])[CH:30]=[CH:29][C:18]=1[C:19]([C:21]1[CH:22]=[CH:23][C:24]([CH2:25][S:1][C:2]2[N:3]([CH3:12])[C:4](=[O:11])[C:5]3[S:10][CH:9]=[CH:8][C:6]=3[N:7]=2)=[CH:27][CH:28]=1)=[O:20]
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참가 물질

6

반응물 3

HCID 189192794-(2,4-Dichlorobenzoyl)benzyl bromideHCID 23719242Sodium hydroxide--water (1/1/1)HCID 178481668HCID 178481668, 화합물

생성물 1

HCID 189191202-[4-(2,4-Dichlorobenzoyl)benzylthio]-3-methylthieno[3,2-d]pyrimidin-4(3H)-one수율 72.6%

시약·촉매·용매 2

HCID 702Ethanol용매
HCID 962
Water
용매

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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 (5.5 ml) in ethanol (20 ml) was added 4-(2,4-dichlorobenzoyl)benzyl bromide (1.91 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 to provide the title compound as colorless solid (1.69 g).

후처리

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

출처 및 근거

ORD 기록
ord-73afaed5e3824cea8d73b23fbdf4f62c
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753664

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