Mesityl oxide → Piperitenone

HRID 1251624

반응식

HRID 1251624 반응식
[O:1]=[C:2]([CH:4]=[C:5]([CH3:7])[CH3:6])[CH3:3].[OH-].[CH2:9]([N+](C)(C)C)[C:10]1C=CC=C[CH:11]=1.O[CH2:21]CC(=O)C>C(O)(=O)C>[CH3:6][C:5]1[CH2:7][CH2:21][C:3](=[C:10]([CH3:11])[CH3:9])[C:2](=[O:1])[CH:4]=1

참가 물질

5

반응물 3

HCID 8858Mesityl oxideHCID 66854Benzyltrimethylammonium hydroxideHCID 1115094-Hydroxy-2-Butanone

생성물 1

HCID 381152Piperitenone수율 60%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
80 °C

실험 절차

A 688 ml (6.0 mol) portion of mesityl oxide was put into a one liter capacity four neck flask, 4.18 ml (10 mmol) of 40% benzyltrimethylammonium hydroxide aqueous solution was added dropwise thereto and the mixture was heated to 80° C. To this was added dropwise 172 ml (2.0 mol) of 4-hydroxy-2-butanone spending 1 hour while keeping at 80° C. After completion of the dropwise addition, this was stirred for 30 minutes and then neutralized by adding dropwise 0.69 ml of acetic acid. By carrying out distillation of the reaction solution under a reduced pressure, 180 g of piperitenone was obtained. Yield 60%.

후처리

  1. additionwas added dropwise
  2. customwhile keeping at 80° C
  3. additionAfter completion of the dropwise addition
  4. distillationdistillation of the reaction solution under a reduced pressure

출처 및 근거

ORD 기록
ord-83d1826d5c254b6890b0878c2d831240
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06342644B1

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