4-(Acetyloxy)-2-butanone → 2,3,6-Trimethylcyclohex-2-en-1-one
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
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
- customare dripped in the course of one hour
- customfrom separate supply vessels
- temperatureThe whole is then heated
- temperatureunder reflux for another hour
- filtrationDeposited sodium acetate is filtered off
- 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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