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Lawesson's reagent → HCID 58423943, 화합물

HRID 1408638
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HRID 1408638 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:11]3([C:15](=[O:16])[NH:14][C:13](=O)[NH:12]3)[CH2:10][CH:9]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[O:8][C:5]2=[CH:6][CH:7]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:33])=CC=1>O1CCOCC1>[Br:1][C:2]1[CH:3]=[C:4]2[C:11]3([C:15](=[O:16])[NH:14][C:13](=[S:33])[NH:12]3)[CH2:10][CH:9]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[O:8][C:5]2=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 58423847HCID 58423847, 화합물

생성물 1

HCID 58423943HCID 58423943, 화합물수율 67%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A suspension of 6-bromo-2-phenylspiro[chroman-4,4′-imidazolidine]-2′,5′-dione (1.12 g, 3 mmol) and Lawesson's Reagent (1.21 g, 3 mmol) in dry 1,4-dioxane (25 mL) was refluxed for 24 h. The mixture was concentrated in vacuo and the residue was purified by preparative TLC to give 6-bromo-2-phenyl-2′-thioxospiro[chroman-4,4′-imidazolidin]-5′-one (780 mg, 67%). 1H-NMR (CDCl3): 2.26 (dd, 1H), 2.43 (dd, 1H), 5.76 (dd, 1H), 6.84 (m, 2H), 7.32-7.36 (m, 6H), 8.22 (m, 1H).

후처리

  1. temperaturewas refluxed for 24 h
  2. concentrationThe mixture was concentrated in vacuo
  3. customthe residue was purified by preparative TLC

출처 및 근거

ORD 기록
ord-e55e418bf8bd4d10a75ba6ac659d6545
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921359B2

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