HCID 14249478, 화합물 → alpha-(Aminomethyl)-2,2-dimethyl-1,3-dioxolane-4-methanol
반응식
[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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-0c3b4fdca9894b64bbf5b91d26572317
- 출처 데이터셋
- uspto-grants-1986_02
- 특허 번호
- US04570007
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