Thiophenol → 2-Chloro-4-(phenylthio)pyrimidine

HRID 577392

반응식

HRID 577392 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.[Na].[C:10]1([SH:16])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C(O)C.C(OCC)(=O)C>[Cl:1][C:2]1[N:7]=[C:6]([S:16][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:5]=[CH:4][N:3]=1

참가 물질

6

반응물 3

HCID 7969ThiophenolHCID 775312,4-DichloropyrimidineHCID 5360545Sodium

생성물 1

HCID 219952052-Chloro-4-(phenylthio)pyrimidine수율 36%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a stirred solution of 2,4-dichloropyrimidine (1.00 g, 6.71 mmol) in absolute ethanol (10 mL), was added sodium salt of benzenethiol (0.89 g, 6.73 mmol)in small portions. The mixture was stirred at room temperature for 2 hours, then at 40° C. for 16 hours. It was diluted with ethyl acetate (20 mL), and filtered. The filtrate was concentrated in vacuo, and the residue was flash chromatographed on silica gel using ethyl acetate:petroleum ether (1:99→25:75) as eluant to give the desired product (498 mg, 36%).

후처리

  1. waitat 40° C. for 16 hours
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated in vacuo
  4. customchromatographed on silica gel

출처 및 근거

ORD 기록
ord-3ed04ce3ef9b4af6adf98607be7aa7e5
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040549B2

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