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Dimethylformamide → HCID 13393792, 화합물

HRID 2107722
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HRID 2107722 반응식
[CH3:1][O:2][C:3]1[C:12]([O:13][CH3:14])=[C:11]([O:15][CH3:16])[CH:10]=[C:9]2[C:4]=1[C:5](=O)[CH2:6][CH:7]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[O:8]2.P(Cl)(Cl)([Cl:26])=O.CN(C)[CH:31]=[O:32]>>[Cl:26][C:5]1[C:4]2[C:9](=[CH:10][C:11]([O:15][CH3:16])=[C:12]([O:13][CH3:14])[C:3]=2[O:2][CH3:1])[O:8][CH:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:6]=1[CH:31]=[O:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 124051375,6,7-Trimethoxy-2-phenyl-2,3-dihydro-4H-1-benzopyran-4-one

생성물 1

HCID 13393792HCID 13393792, 화합물

실험 절차

As in example 1, but using 15 g 5,6,7-trimethoxyflavanone, 150 ml dimethylformamide and 26 ml phosphorous oxychloride. Reaction time is forty eight hours at room temperature. After hydrolysis and usual work up, the residual solid is purified by preparative HPLC and the best fractions are crystallised in hexane. 4-chloro-3-formyl-5,6,7-trimethoxyflav-3-ene is obtained as yellow crystals; m.p. 84°-87° C.

후처리

  1. customReaction time
  • waitis forty eight hours at room temperature
  • customAfter hydrolysis and usual work up
  • customthe residual solid is purified by preparative HPLC
  • customthe best fractions are crystallised in hexane
  • 출처 및 근거

    ORD 기록
    ord-3f2c4f1dea9a4de7846c1472f60509c2
    출처 데이터셋
    uspto-grants-1990_06
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04935441

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