Thionyl Chloride → Ethyl (2-chloro-6-oxocyclohex-1-en-1-yl)acetate
反応式
O.[O:2]=[C:3]1[CH2:8][CH2:7][CH2:6][C:5](=O)[CH:4]1[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12].S(Cl)([Cl:18])=O>C(Cl)Cl>[Cl:18][C:5]1[CH2:6][CH2:7][CH2:8][C:3](=[O:2])[C:4]=1[CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12]参加物
4
実験手順
A slurry of ethyl α-(2,6-dioxocyclohexyl)acetate hydrate (1.53 kg) in methylene chloride (7.7 L) is brought to reflux and then thionyl chloride (1.80 kg) is added dropwise over a period of 1.75 hours. The solution is refluxed for 3 hours and then evaporated in vacuo to yield an oil which is distilled to give ethyl α-(2-chloro-6-oxo-cyclohex-1-enyl)acetate as a yellow oil, bp 115°-125°/0.2 mm.
後処理
- temperatureto reflux
- temperatureThe solution is refluxed for 3 hours
- customevaporated in vacuo
- customto yield an oil which
- distillationis distilled
出典と根拠
- ORDレコード
- ord-4cecf2364d054435b86a7d41f0fce6f0
- 出典データセット
- uspto-grants-1991_02
- 特許番号
- US04992465
反応ノート
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