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4-(6-Chloronicotinoyl)benzyl bromide → 2-[4-(6-Chloronicotinoyl)benzylthio]-3-methylthieno[3,2-d]pyrimidin-4(3H)-one

HRID 1291347
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HRID 1291347 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]=[CH:31][C:20]([C:21]([C:23]2[CH:30]=[CH:29][C:26]([CH2:27]Br)=[CH:25][CH:24]=2)=[O:22])=[CH:19][N:18]=1>C(O)C.O>[Cl:16][C:17]1[CH:32]=[CH:31][C:20]([C:21]([C:23]2[CH:30]=[CH:29][C:26]([CH2:27][S:1][C:2]3[N:3]([CH3:12])[C:4](=[O:11])[C:5]4[S:10][CH:9]=[CH:8][C:6]=4[N:7]=3)=[CH:25][CH:24]=2)=[O:22])=[CH:19][N:18]=1
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참가 물질

6

반응물 3

HCID 189188004-(6-Chloronicotinoyl)benzyl bromideHCID 23719242Sodium hydroxide--water (1/1/1)HCID 178481668HCID 178481668, 화합물

생성물 1

HCID 189187982-[4-(6-Chloronicotinoyl)benzylthio]-3-methylthieno[3,2-d]pyrimidin-4(3H)-one수율 74.7%

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 (1.98 g) and 1N-sodium hydroxide/water (10.5 ml) in ethanol (30 ml) was added 4-(6-chloronicotinoyl)benzyl bromide (3.35 g) and the mixture was stirred at 60° C. fro 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 light-yellow solid (3.194 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-df96414ab3f6453bbb652154ff97026a
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753664

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