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Benzene → 7,8-Diacetoxychromone-3-carbonyl chloride

HRID 1649123
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HRID 1649123 반응식
[C:1]([O:4][C:5]1[C:14]([O:15][C:16](=[O:18])[CH3:17])=[C:13]2[C:8]([C:9](=[O:22])[C:10]([C:19](O)=[O:20])=[CH:11][O:12]2)=[CH:7][CH:6]=1)(=[O:3])[CH3:2].S(Cl)([Cl:25])=O.C1C=CC=CC=1>CN(C)C=O>[C:1]([O:4][C:5]1[C:14]([O:15][C:16](=[O:18])[CH3:17])=[C:13]2[C:8]([C:9](=[O:22])[C:10]([C:19]([Cl:25])=[O:20])=[CH:11][O:12]2)=[CH:7][CH:6]=1)(=[O:3])[CH3:2]
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참가 물질

5

반응물 3

HCID 241BenzeneHCID 24386Thionyl Chloride2회HCID 127658457,8-Diacetoxychromone-3-carboxylic acid

생성물 1

HCID 541479727,8-Diacetoxychromone-3-carbonyl chloride

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A mixture of 7,8-diacetoxychromone-3-carboxylic acid (9.5 g), thionyl chloride (2.6 ml), dimethylformamide (0.1 ml) and benzene (300 ml) was refluxed for one and half hours, and there were further added thionyl chloride (2.6 ml) and dimethyl formamide (0.1 ml). The whole was then refluxed for further one hour. Then the solvent was removed therefrom by distillation, and the residue was triturated with n-bexane. The solid matter thus obtained was collected by filtration. There was thus obtained the desired product (9.3 g).

후처리

  1. temperaturewas refluxed for one and half hours, and there
  2. temperatureThe whole was then refluxed for further one hour
  3. customThen the solvent was removed
  4. distillationby distillation
  5. customthe residue was triturated with n-bexane
  6. customThe solid matter thus obtained
  7. filtrationwas collected by filtration

출처 및 근거

ORD 기록
ord-22eac24062ad4e9ba370372699c431ac
출처 데이터셋
uspto-grants-1983_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04415567

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