HCID 14249478、化合物 → alpha-(Aminomethyl)-2,2-dimethyl-1,3-dioxolane-4-methanol
反応式
[N:1]([CH2:4][CH:5]([CH:7]1[CH2:11][O:10][C:9]([CH3:13])([CH3:12])[O:8]1)[OH:6])=[N+]=[N-]>CO.[Pd]>[NH2:1][CH2:4][CH:5]([CH:7]1[CH2:11][O:10][C:9]([CH3:13])([CH3:12])[O:8]1)[OH:6]参加物
4
実験手順
A solution of 9.36 g of 2-azido-1-(2,2,-dimethyl-1,3-dioxolan-4-yl)ethanol in 150 ml of methanol is combined with 900 mg of palladium/charcoal catalyst (10%). The hydrogenation is conducted for 1 hour under normal pressure. The mixture is then filtered off from the catalyst and washed with methanol. The combined solutions are concentrated to dryness under vacuum. The remaining oil is crystallized from ethanol/ether, thus obtaining 6.29 g (78% of theory) of 2-amino-1-(2,2-dimethyl-1,3-dioxolan-4-yl)ethanol in white needles, mp 94°-96° C.
後処理
- filtrationThe mixture is then filtered off from the catalyst
- washwashed with methanol
- concentrationThe combined solutions are concentrated to dryness under vacuum
- customThe remaining oil is crystallized from ethanol/ether
出典と根拠
- ORDレコード
- ord-0c3b4fdca9894b64bbf5b91d26572317
- 出典データセット
- uspto-grants-1986_02
- 特許番号
- US04570007
反応ノート
読み込み中…