HCID 642972、化合物 → HCID 12728388、化合物
反応式
[CH3:1][C:2]1[CH2:11][C:6]2([CH2:10][CH2:9][CH2:8][CH2:7]2)[O:5][CH2:4][CH:3]=1.[H][H]>[Ni].[Pd].C(O)(C)C>[CH3:1][CH:2]1[CH2:11][C:6]2([CH2:7][CH2:8][CH2:9][CH2:10]2)[O:5][CH2:4][CH2:3]1参加物
6
実験手順
A solution of 9-methyl-6-oxaspiro[4.5]dec-8-ene (1.52 kg, 10.0 mols), isopropyl alcohol (1000 ml) and Raney nickel (100 g), Pd/C (100 g) or other suitable sponge-metal catalyst was hydrogenated at 450 psi, at 140° C. for 10-12 h until the theoretical amount of hydrogen was taken up. The mixture was cooled and filtrated. The isopropyl alcohol was evaporated and the residue obtained was distilled under reduced pressure to provide 9-methyl-6-oxaspiro[4.5]decane (1.4 kg, yield: 95%, purity: 98%).
後処理
- temperatureThe mixture was cooled
- filtrationfiltrated
- customThe isopropyl alcohol was evaporated
- customthe residue obtained
- distillationwas distilled under reduced pressure
出典と根拠
- ORDレコード
- ord-eb70911fa5bd4d23b969e97fc3bb020c
- 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…