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

HRID 67098
ノート
印刷プレビュー

反応式

HRID 67098 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

6,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carboxylic acid (57.3 mg) was dissolved in benzene (10 ml). To the solution was added with stirring at room temperature thionyl chloride (0.5 ml). The mixture was refluxed with stirring for three hours, and the reaction solution was concentrated. To the concentrate was added n-hexane (5 ml) to cause crystallization of the reaction product. The resulting product was recovered by filtration and washed with n-hexan and dried. There were thus obtained 34.8 mg of the desired product (34.8 mg).

後処理

  1. additionTo the solution was added
  2. temperatureThe mixture was refluxed
  3. concentrationthe reaction solution was concentrated
  4. additionTo the concentrate was added n-hexane (5 ml)
  5. customcrystallization of the reaction product
  6. filtrationThe resulting product was recovered by filtration
  7. washwashed with n-hexan
  8. customdried

出典と根拠

ORDレコード
ord-1d512c92792f43509a09120bf02ffcbe
出典データセット
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04344944

反応ノート

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