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Thionyl Chloride → 6,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carbonyl chloride

HRID 1105533
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HRID 1105533 반응식
[Cl:1][C:2]([Cl:32])([Cl:31])[CH2:3][O:4][C:5]([O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][C:17]=1[O:18][C:19]([O:21][CH2:22][C:23]([Cl:26])([Cl:25])[Cl:24])=[O:20])[O:14][CH:13]=[C:12]([C:27]([OH:29])=O)[C:11]2=[O:30])=[O:6].S(Cl)([Cl:35])=O>C1C=CC=CC=1>[Cl:1][C:2]([Cl:31])([Cl:32])[CH2:3][O:4][C:5]([O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][C:17]=1[O:18][C:19]([O:21][CH2:22][C:23]([Cl:26])([Cl:24])[Cl:25])=[O:20])[O:14][CH:13]=[C:12]([C:27]([Cl:35])=[O:29])[C:11]2=[O:30])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 128006276,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carboxylic acid

생성물 1

HCID 128006286,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carbonyl chloride

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

The compound (57.3 mg) obtained in Example 5 was dissolved in 10 ml of benzene, and with stirring at room temperature, 0.5 ml of thionyl chloride was added. The mixture was refluxed for 3 hours with stirring. The reaction mixture was concentrated, and 5 ml of n-hexane was added to the concentrate to crystallize it. The resulting crystals were collected by filtration, washed with n-hexane and dried to afford 34.8 mg of the desired product.

후처리

  1. temperatureThe mixture was refluxed for 3 hours
  2. stirringwith stirring
  3. concentrationThe reaction mixture was concentrated
  4. addition5 ml of n-hexane was added to the
  5. concentrationconcentrate
  6. customto crystallize it
  7. filtrationThe resulting crystals were collected by filtration
  8. washwashed with n-hexane
  9. customdried

출처 및 근거

ORD 기록
ord-cd2d912029eb4d2d90935399b209fd23
출처 데이터셋
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04309354

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