Acetyl chloride → HCID 18423181、化合物

HRID 2260566ノート

反応式

HRID 2260566 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[CH3:5][C:6]([NH:14][C:15](=[O:17])[CH3:16])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[CH3:7].[C:18](Cl)(=[O:20])[CH3:19]>ClC(Cl)C>[C:18]([C:11]1[CH:10]=[CH:9][C:8]([C:6]([NH:14][C:15](=[O:17])[CH3:16])([CH3:5])[CH3:7])=[CH:13][CH:12]=1)(=[O:20])[CH3:19]

参加物

5

反応物 3

HCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 10749810N-(2-phenylpropan-2-yl)acetamide

生成物 1

HCID 18423181HCID 18423181、化合物収率 66%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

Aluminum chloride (41.5 g) was portionwise added to a solution (75 ml) of N-(1-methyl-1-phenylethyl)acetamide (25 g) and acetyl chloride (16.6 g) in dichloroethane under ice-cooling. The mixture was stirred at said temperature for 1 hour and then at 50°-60° C. for 1 hour. After completion of the reaction, the reaction mixture was poured into ice water and extracted with chloroform. The extract was washed with water, dried and concentrated under reduced pressure to give crystals which were then recrystallized from ethyl acetate-isopropyl ether to give 20.4 g of N-(1-(4-acetylphenyl)-1-methylethyl)acetamide.

後処理

  1. temperaturecooling
  2. customfor 1 hour
  3. customAfter completion of the reaction
  4. extractionextracted with chloroform
  5. washThe extract was washed with water
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customto give crystals which
  9. customwere then recrystallized from ethyl acetate-isopropyl ether

出典と根拠

ORDレコード
ord-a5a1bba2bce64818b2e7422e8fcfc918
出典データセット
uspto-grants-1995_12
特許番号
US05478838

反応ノート

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