反応式
Cl[C:2]1[CH2:7][C:6]([CH3:9])([CH3:8])[CH2:5][C:4](=[O:10])[CH:3]=1.[I-].[K+]>CO.[Zn]>[CH3:8][C:6]1([CH3:9])[CH2:5][C:4](=[O:10])[CH:3]=[CH:2][CH2:7]1参加物
5
実験手順
Activated zinc dust (15.0 g) was added to a stirred solution of 3-chloro-5,5-dimethylcyclohex-2-enone (9.0 g) and potassium iodide (7.5 g) in methanol (50 ml). After stirring for a period of 18 hours the mixture was filtered and the filtrate concentrated by evaporation under reduced pressure. The residue was mixed with dilute (8% w/v) hydrochloric acid and extracted with diethyl ether (2 × 100 ml). The combined ethereal extracts were washed with water and dried over anhydrous magnesium sulphate. After removal of the ether by evaporation under reduced pressure the residual oil was purified by distillation. 5,5-Dimethylcyclohex-2-enone was obtained as a pale yellow oil, b.p. 75° C./17 mm Hg.
後処理
- filtrationwas filtered
- concentrationthe filtrate concentrated by evaporation under reduced pressure
- additionThe residue was mixed
- additionwith dilute (8% w/v) hydrochloric acid
- extractionextracted with diethyl ether (2 × 100 ml)
- washThe combined ethereal extracts were washed with water
- dry with materialdried over anhydrous magnesium sulphate
- customAfter removal of the ether
- customby evaporation under reduced pressure the residual oil
- distillationwas purified by distillation
出典と根拠
- ORDレコード
- ord-ed4bcaa9561f4a89969a56d4bc50453d
- 出典データセット
- uspto-grants-1978_07
- 特許番号
- US04102896
関連ノート
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