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Benzoyl chloride → 6-Hydroxy-7-benzoyl-1,2,3,4-tetrahydro-1-naphthylacetic acid ethyl ester

HRID 1680281
ノート
印刷プレビュー

反応式

HRID 1680281 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[CH2:5]([O:7][C:8](=[O:22])[CH2:9][CH:10]1[C:19]2[C:14](=[CH:15][C:16]([O:20]C)=[CH:17][CH:18]=2)[CH2:13][CH2:12][CH2:11]1)[CH3:6].[C:23](Cl)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C(Cl)Cl>[CH2:5]([O:7][C:8](=[O:22])[CH2:9][CH:10]1[C:19]2[C:14](=[CH:15][C:16]([OH:20])=[C:17]([C:23](=[O:30])[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:18]=2)[CH2:13][CH2:12][CH2:11]1)[CH3:6]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7412Benzoyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 13420659Ethyl 2-(6-methoxy-1,2,3,4-tetrahydronaphthalen-1-yl)acetate

生成物 1

HCID 540031226-Hydroxy-7-benzoyl-1,2,3,4-tetrahydro-1-naphthylacetic acid ethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
5 °C

実験手順

26.6 g of finely powdered aluminium chloride are added in portions to a solution of 10 g of 6-methoxy-1,2,3,4-tetrahydro-1-naphthyl-acetic acid ethyl ester in 50 ml of absolute methylene chloride whilst stirring at 5° C., and thereafter 16.9 g of benzoyl chloride are added sufficiently slowly that the reaction solution boils gently under reflux. After completion of the addition, the reaction mixture is allowed to boil for a further 30 minutes and is then allowed to cool to room temperature, after which it is poured onto 300 g of ice. The mixture is extracted with 3 times 100 ml of methylene chloride and the organic phases are washed until neutral, dried over sodium sulphate and evaporated to dryness in vacuo. Chromatography of the evaporation residue on 500 g of silica gel, using methylene chloride as the eluting agent, gives 6-hydroxy-7-benzoyl-1,2,3,4-tetrahydro-1-naphthylacetic acid ethyl ester of boiling point 190° C./0.04 mm Hg.

後処理

  1. temperatureunder reflux
  2. additionAfter completion of the addition
  3. temperatureto cool to room temperature
  4. extractionThe mixture is extracted with 3 times 100 ml of methylene chloride
  5. washthe organic phases are washed until neutral,
  6. dry with materialdried over sodium sulphate
  7. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-781caa7872a74ced886629926304a523
出典データセット
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04272547

反応ノート

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