p-Toluenesulfonic acid → HCID 642972、化合物
反応式
[CH3:1][C:2]1[CH:3]=CC(S(O)(=O)=O)=[CH:6][CH:7]=1.[C:12]1(=[O:17])[CH2:16][CH2:15][CH2:14][CH2:13]1.CC(CCO)=C>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH2:3][C:12]2([CH2:16][CH2:15][CH2:14][CH2:13]2)[O:17][CH2:6][CH:7]=1参加物
5
反応条件
- 温度
- 115 °C
実験手順
A mixture of p-TSA (20 g, 0.105 mol) and toluene (2 L) was heated to 115° C. To this mixture were added cyclopentanone (840 g, 10 mols) and isoprenol (946 g, 11 mols) and heated further for 3-6 h. Water was removed from the reaction azeotropically. The reaction mixture was then cooled to room temperature. The organic phase was washed with a 5% Na2CO3 solution, washed with water dried and concentrated and distilled further to provideto 9-methyl-6-oxaspiro[4.5]dec-8-ene (0.851 kg) having a purity of 95% (sum of the isomers) for a total yield of 56%.
後処理
- temperatureheated further for 3-6 h
- customWater was removed from the reaction azeotropically
- temperatureThe reaction mixture was then cooled to room temperature
- washThe organic phase was washed with a 5% Na2CO3 solution
- washwashed with water
- customdried
- concentrationconcentrated
- distillationdistilled further
出典と根拠
- ORDレコード
- ord-3f9a1549855c4b0584c8073fd88b0155
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09187709B2
反応ノート
読み込み中…