反応式
[CH:1]1([CH2:8][CH2:9][C:10]#[N:11])[CH2:6][CH2:5][CH2:4][CH2:3][C:2]1=[O:7].ClC1C=CC=C(C(OO)=[O:20])C=1.[Cl:23][C:24]1[CH:25]=[C:26]([CH:30]=[CH:31][CH:32]=1)[C:27]([OH:29])=[O:28]>CCCCCC>[C:10]([CH2:9][CH2:8][CH:1]1[O:20][C:2](=[O:7])[CH2:3][CH2:4][CH2:5][CH2:6]1)#[N:11].[Cl:23][C:24]1[CH:25]=[C:26]([CH:30]=[CH:31][CH:32]=1)[C:27]([OH:29])=[O:28]参加物
反応条件
- 温度
- 55 °C
実験手順
A reactor is loaded with 151 g of 3-(2-cyclohexanonyl)propionitrile in 500 ml of n-hexane and 260 g of m-chloroperbenzoic acid (70% titer) dissolved at 50° C. in 2000 ml of n-hexane in 30 minutes. The solution is heated to 55° C. for 15 hours. Cooling of the solution separates, in crystalline form, part of the m-chlorobenzoic acid which is scarcely soluble in the system, together with a heavy liquid phase which is formed by 7-cyanoethyl-2-oxepanone and by m-chlorobenzoic acid. 71.5 g of 7-cyanoethyl-2-oxepanone, impure with m-chlorobenzoic acid, are recovered from the lower phase. 24 g of 7-cyanoethyl-2-oxepanone are recovered from the upper phase by concentration and several crystallizations. Conversion over the initial ketone is 85%. Yield on the converted amount is 57%.
出典と根拠
- ORDレコード
- ord-08b32fbbc1ad4e3a8e50204892016904
- 出典データセット
- uspto-grants-1999_02
- 特許番号
- US05872267
関連ノート
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