4-(Acetyloxy)-2-butanone → 2,3,6-Trimethylcyclohex-2-en-1-one

HRID 65808노트

반응식

HRID 65808 반응식
C(O[CH2:5][CH2:6][C:7](=O)[CH3:8])(=O)C.[CH3:10][O-:11].[Na+]>CO>[CH3:5][C:6]1[C:10](=[O:11])[CH:7]([CH3:8])[CH2:6][CH2:5][C:7]=1[CH3:8]

참가 물질

4

반응물 2

HCID 1391004-(Acetyloxy)-2-butanoneHCID 10942334Sodium Methoxide

생성물 1

HCID 30168432,3,6-Trimethylcyclohex-2-en-1-one

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

130 g of 1-acetoxybutan-3-one and sodium methylate solution in methanol are dripped in the course of one hour from separate supply vessels while stirring into 400 g of boiling diethyl ketone at such a rate that the reaction mixture remains constantly alkaline. A total of 190 g of a 30% by weight sodium methylate solution is used up in this way. The whole is then heated under reflux for another hour and then neutralized with glacial acetic acid. Deposited sodium acetate is filtered off and the filtrate is subjected to fractional distillation. 81 g of 2,3,6-trimethyl-2-cyclohexen-1-one is obtained as well as traces of 4-methyl-3-ethyl-2-cyclohexen-1-one. The yield with reference to 1-acetoxybutan-3-one is 59%.

후처리

  1. customare dripped in the course of one hour
  2. customfrom separate supply vessels
  3. temperatureThe whole is then heated
  4. temperatureunder reflux for another hour
  5. filtrationDeposited sodium acetate is filtered off
  6. distillationthe filtrate is subjected to fractional distillation

출처 및 근거

ORD 기록
ord-6378b9e4c99d40c6811d8c8750d9496a
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04128728

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