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5-Chloro-2(1H)-pyrimidinone → 5-Chloro-1-(4-methylthiophenacyl)pyrimidin-2-one

HRID 980177
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HRID 980177 반응식
[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[NH:6][CH:7]=1.Br[CH2:10][C:11]([C:13]1[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=1)=[S:12]>C(N(CC)CC)C.C(O)C>[Cl:1][C:2]1[CH:3]=[N:4][C:5](=[O:8])[N:6]([CH2:10][C:11]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=2)=[S:12])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 1085785-Chloro-2(1H)-pyrimidinoneHCID 183681522-Bromo-4'-methylthioacetophenone

생성물 1

HCID 537912715-Chloro-1-(4-methylthiophenacyl)pyrimidin-2-one수율 63.3%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8471Triethylamine용매

실험 절차

A suspension of 5-chloropyrimidin-2-one (312 mg) and 2-bromo-4'-methylthioacetophenone (525 mg) in triethylamine (1 ml) and ethanol (20 ml) was stirred at ambient temperature for 2.25 hours. The resulting suspension was concentrated at reduced pressure then diluted with water (50 ml). The collected precipitate was crystallised from acetone to give the title pyrimidinone (404 mg,); m.p. 192°-197°, λmaxEtOH 229 nm (ε 14450), 312 nm (ε 21470), λinf 239.5 nm (ε 9930).

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후처리

  1. concentrationThe resulting suspension was concentrated at reduced pressure
  2. additionthen diluted with water (50 ml)
  3. customThe collected precipitate was crystallised from acetone

출처 및 근거

ORD 기록
ord-bf3f0cab3246439a8dc2f70650dcfbf8
출처 데이터셋
uspto-grants-1987_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04636509

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