反応式
[CH2:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([CH:10]2[CH2:15][CH2:14][C:13](=O)[CH2:12][CH2:11]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3].[NH:17]1[CH2:21][CH2:20][CH2:19][CH2:18]1.O>C1(C)C=CC=CC=1>[CH2:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([CH:10]2[CH2:15][CH2:14][C:13]([N:17]3[CH2:21][CH2:20][CH2:19][CH2:18]3)=[CH:12][CH2:11]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3]参加物
実験手順
200 g of 4-(trans-4-propylcyclohexyl)cyclohexanone and 135.2 g of pyrrolidine were dissolved in 800 ml of toluene. The solution was heated and stirred for 6 hours while water which is evaporated by azeotropic distillation was removed. Azeotropic distillation of the solution was carried out with toluene so that excessive pyrrolidine was removed, and 1-(4-(trans-4-propylcyclohexyl)-cyclohexen-1-yl)-pyrrolidine was obtained. The product as it was was cooled to room temperature, and 800 ml of toluene was added again. The mixture was cooled in a water bath, and 150 ml toluene solution of 89 ml of methyl vinyl ketone was added dropwise over a period of 2 hours at 20° C. or less. After the dropwise addition was completed, the temperature was increased over a period of 2 hours to reach the reflux temperature. The solution was cooled to room temperature, and a buffer solution of pH 5 which was prepared from B5.2 g of sodium acetate, 104.2 ml of acetic acid, and 104.2 ml of water was added. Reflux was further continued for 5 hours. After the solution was cooled to room temperature, the organic phase was separated and rinsed with water and a saturated saline solution. The organic phase was dried on anhydrous sodium sulfate. The solvent was evaporated, and 313 g of 6-(trans-4-propylcyclohexyl)-4,4a,5,6,7,8-hexahydro-2(3H)-naphthalenone was obtained.
後処理
- temperatureThe solution was heated
- customis evaporated by azeotropic distillation
- customwas removed
- distillationAzeotropic distillation of the solution
- customwas removed
出典と根拠
- ORDレコード
- ord-fe6957f798684a7abfc8c152170636a4
- 出典データセット
- uspto-grants-2005_07
- 特許番号
- US06913797B1
関連ノート
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