Acetyl chloride → 1-(2,3-Dihydro-1,1,2,3,3-pentamethyl-1H-inden-5-yl)ethan-1-one

HRID 1111546

反応式

HRID 1111546 の反応式
[CH3:1][C:2]1([CH3:14])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([CH3:12])([CH3:11])[CH:3]1[CH3:13].[C:15](Cl)(=[O:17])[CH3:16].[Cl-].[Al+3].[Cl-].[Cl-]>>[C:15]([C:8]1[CH:9]=[C:10]2[C:5](=[CH:6][CH:7]=1)[C:4]([CH3:12])([CH3:11])[CH:3]([CH3:13])[C:2]2([CH3:14])[CH3:1])(=[O:17])[CH3:16]

参加物

4

反応物 3

HCID 6367Acetyl chlorideHCID 145491,1,2,3,3-PentamethylindanHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 1073331-(2,3-Dihydro-1,1,2,3,3-pentamethyl-1H-inden-5-yl)ethan-1-one

実験手順

To a mixture, stirred at ambient temperature in the absence of the humidity of the air, of 25 g of 1,1,2,3,3-pentamethyl indane and 13 cm3 of acetyl chloride, there are added, in small portions, 23 g of aluminum chloride in a manner such that the temperature does not exceed 40° C. Stirring is maintained for 2 hours after the end of the addition and the reaction mixture is left overnight. The next day, it is poured into 200 cm3 of ice water and then extracted three times with 150 cm3 of dichloromethane. The organic phases are combined, washed with sodium bicarbonate and then with water and dried on magnesium sulfate. The solvent is removed by evaporation under a vacuum and 31 g of 5-acetyl-1,1,2,3,3-pentamethyl indane in liquid form which is directly used for the following reactions are obtained.

後処理

  1. customdoes not exceed 40° C
  2. temperatureis maintained for 2 hours
  3. additionafter the end of the addition
  4. extractionextracted three times with 150 cm3 of dichloromethane
  5. washwashed with sodium bicarbonate
  6. dry with materialwith water and dried on magnesium sulfate
  7. customThe solvent is removed by evaporation under a vacuum and 31 g of 5-acetyl-1,1,2,3,3-pentamethyl indane in liquid form which
  8. customare obtained

出典と根拠

ORDレコード
ord-7f9cbff27c134d79bfc4decf39a258d2
出典データセット
uspto-grants-1990_12
特許番号
US04980509

関連ノート

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