Methyl vinyl ketone → Piperitenone

HRID 1251626

反応式

HRID 1251626 の反応式
[O:1]=[C:2]([CH:4]=[C:5]([CH3:7])[CH3:6])[CH3:3].[C:8](=O)([O-])[O-].[K+].[K+].[CH:14]([C:16](C)=O)=[CH2:15]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1>[CH3:6][C:5]1[CH2:7][CH2:8][C:3](=[C:14]([CH3:16])[CH3:15])[C:2](=[O:1])[CH:4]=1

参加物

5

反応物 3

HCID 6570Methyl vinyl ketoneHCID 8858Mesityl oxideHCID 11430Potassium Carbonate

生成物 1

HCID 381152Piperitenone収率 62%

試薬・触媒・溶媒 1

HCID 66133Benzyl triethylammonium chloride触媒

反応条件

温度
80 °C

実験手順

A 688 ml (6.0 mol) portion of mesityl oxide was put into a one liter capacity four neck flask and mixed with 13.82 g (0.1 mol) of potassium carbonate and 2.28 g (10 mmol) of benzyltriethylammonium chloride, and the mixture was heated to 80° C. To this was added dropwise 166.48 ml (2.0 mol) of methyl vinyl ketone spending 1 hour while keeping at 80° C. After completion of the dropwise addition, this was stirred for 30 minutes and then the reaction solution was distilled under a reduced pressure to obtain 186 g of piperitenone. Yield 62%.

後処理

  1. customwhile keeping at 80° C
  2. additionAfter completion of the dropwise addition
  3. distillationthe reaction solution was distilled under a reduced pressure

出典と根拠

ORDレコード
ord-d2d191a2702e4faa9c85cb404e4a74d9
出典データセット
uspto-grants-2002_01
特許番号
US06342644B1

関連ノート

読み込み中…