Hydrogen Bromide → HCID 10243700、化合物
反応式
Br.Cl.C[O:4][C:5]1[CH:6]=[CH:7][C:8]2[O:21][CH2:20][C@H:12]3[N:13]([CH2:17][CH2:18][CH3:19])[CH2:14][CH2:15][CH2:16][C@@H:11]3[C:9]=2[CH:10]=1>>[OH:4][C:5]1[CH:6]=[CH:7][C:8]2[O:21][CH2:20][C@H:12]3[N:13]([CH2:17][CH2:18][CH3:19])[CH2:14][CH2:15][CH2:16][C@@H:11]3[C:9]=2[CH:10]=1参加物
3
実験手順
A mixture of 21.6 l of 47-49% hydrobromic acid and 2.27 kg of trans-9-methoxy-4-propyl-1,2,3,4a,5,10b-hexahydro-4H-[1]-benzopyrano[3,4-b]pyridine hydrochloride is stirred and heated at 105°-110° for 2 hours. Most of the hydrobromic acid is then removed by distillation (125°/3 mmHg), a solution of 10.5 l of methanol and 9.5 l of water is added and the suspension heated to 75°. The hot mixture is cautiously treated with 2.2 l of 4N sodium hydroxide solution to pH 8, cooled to 10° and filtered. The collected solids are washed five times with 1 l of water each and dried (68°/3 mmHg) to yield trans-9-hydroxy-4-propyl-1,2,3,4a,5,10b-hexahydro-4H-[1]-benzopyrano[3,4-b]pyridine, m.p. 194°-196°.
後処理
- temperatureheated at 105°-110° for 2 hours
- customMost of the hydrobromic acid is then removed by distillation (125°/3 mmHg)
- additiona solution of 10.5 l of methanol and 9.5 l of water is added