Sulfuric acid magnesium salt (1:1) → HCID 12507349、化合物

HRID 728533ノート

反応式

HRID 728533 の反応式
[Cl:1][C:2]1([Cl:11])[C@H:9]2[C@H:4]([CH2:5][CH2:6][CH:7]=[CH:8]2)[C@@H:3]1[OH:10].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)Cl>[Cl:1][C:2]1([Cl:11])[C@H:9]2[C@H:4]([CH2:5][CH2:6][CH:7]=[CH:8]2)[C:3]1=[O:10]

参加物

5

反応物 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 14127271HCID 14127271、化合物HCID 178418287HCID 178418287、化合物

生成物 1

HCID 12507349HCID 12507349、化合物収率 80.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3.9 g of (1R,6S,7S)-8,8-dichlorobicyclo [4.2.0]oct-2-en-7-ol, prepared as shown in Example 1, 9.0 g of pyridinium chlorochromate and 14 g of magnesium sulfate in 200 ml of methylene chloride under nitrogen was refluxed for 4 hours. The mixture was cooled, filtered first through celite then Florisil. Solvent was removed from the eluate under reduced pressure and the residue distilled under vacuum to give 3.1 g of (1R,6S)-8,8-dichlorobicyclo[4.2.0]oct-2-en-7-one, [α]D =+71.4°, (C=0.7, CHCl3).

後処理

  1. customprepared
  2. temperaturewas refluxed for 4 hours
  3. temperatureThe mixture was cooled
  4. filtrationfiltered first through celite
  5. customSolvent was removed from the eluate under reduced pressure
  6. distillationthe residue distilled under vacuum

出典と根拠

ORDレコード
ord-c261590a3987480692eda02152f68240
出典データセット
uspto-grants-1991_09
特許番号
US05049497

反応ノート

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