Acetyl chloride → HCID 20077196、化合物

HRID 1289446ノート

反応式

HRID 1289446 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[CH2:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][CH:6]1[CH2:14][C:15]([O:17][CH3:18])=[O:16].[C:19](Cl)(=[O:21])[CH3:20]>C(Cl)Cl>[C:19]([C:10]1[CH:9]=[C:8]2[C:13](=[CH:12][CH:11]=1)[CH2:5][CH:6]([CH2:14][C:15]([O:17][CH3:18])=[O:16])[CH2:7]2)(=[O:21])[CH3:20]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 14090225Methyl (2,3-dihydro-1H-inden-2-yl)acetate

生成物 1

HCID 20077196HCID 20077196、化合物収率 91%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Added to 160 ml of methylene chloride were 52.9 g (0.388 mol) of anhydrous aluminum chloride. While chilling with ice water, a solution of 25.03 g (0.132 mol) of methyl (indan-2-yl)acetate in 40 ml of methylene chloride was added dropwise to the solution, followed by the addition of 13.1 ml (0.185 mol) of acetyl chloride. After stirring the mixture at the same temperature for 40 minutes, the reaction mixture was poured into ice water to take out an organic layer separated. After the organic layer was washed with water and dried, the solvent was distilled off under reduced pressure. The resultant residue was purified by column chromatography on silica gel (ethyl acetate-hexane=1:2), thereby obtaining 27.8 g of an oily substance. Yield: 91%.

後処理

  1. customseparated
  2. washAfter the organic layer was washed with water
  3. customdried
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe resultant residue was purified by column chromatography on silica gel (ethyl acetate-hexane=1:2)
  6. customobtaining 27.8 g of an oily substance

出典と根拠

ORDレコード
ord-023ea0be0b2840d58d75a70c83a3d725
出典データセット
uspto-grants-1998_05
特許番号
US05750524

反応ノート

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