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Lawesson's reagent → 4,6-Dimethoxy-pyrimidin-2-carbothioic acid amide

HRID 925990
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인쇄 미리보기

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HRID 925990 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([C:11]([NH2:13])=O)[N:4]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:23])=CC=1>C1COCC1>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([C:11](=[S:23])[NH2:13])[N:4]=1
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참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 582826824,6-Dimethoxypyrimidin-2-carboxylic acid amide

생성물 1

HCID 582827014,6-Dimethoxy-pyrimidin-2-carbothioic acid amide수율 72%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
90 °C

실험 절차

To a stirred solution of compound 286 (21.86 g, 1 eq.) in dry THF (200 mL) was added Lawesson's reagent (29 g, 0.6 eq.) under nitrogen. The mixture was then stirred at 90° C. for 1 hr and then concentrated in vacuo. The residue obtained was triturated in a DCM/diisopropyl ether mixture to yield compound 287 as an orange solid in 72% yield. MS (ESI, EI+): m/z=200 (MH+).

후처리

  1. concentrationconcentrated in vacuo
  2. customThe residue obtained
  3. customwas triturated in a DCM/diisopropyl ether mixture

출처 및 근거

ORD 기록
ord-7411267709c04dba8155c5a4978fa968
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09284307B2

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