Hydrochloric Acid → 7-(3-{[(4-methyl-2-pyridinyl)methyl]oxy}-2-pyridinyl)-2,3,4,5-tetrahydro-1H-3-benzazepine
반응식
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([CH2:8][O:9][C:10]2[C:11]([C:16]3[CH:33]=[CH:32][C:19]4[CH2:20][CH2:21][N:22](C(OC(C)(C)C)=O)[CH2:23][CH2:24][C:18]=4[CH:17]=3)=[N:12][CH:13]=[CH:14][CH:15]=2)[CH:3]=1.Cl>O1CCOCC1>[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([CH2:8][O:9][C:10]2[C:11]([C:16]3[CH:33]=[CH:32][C:19]4[CH2:20][CH2:21][NH:22][CH2:23][CH2:24][C:18]=4[CH:17]=3)=[N:12][CH:13]=[CH:14][CH:15]=2)[CH:3]=1참가 물질
4
반응물 2
생성물 1
시약·촉매·용매 1
실험 절차
1,1-dimethylethyl 7-(3-{[(4-methyl-2-pyridinyl)methyl]oxy}-2-pyridinyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (3.8 g) was dissolved in dioxane (20 ml). Gaseous hydrogen chloride was passed through the reaction mixture for 1.5 h. The reaction was monitored by TLC. On completion the solid formed was collected by filtration and washed with acetone. The solid was then dissolved in water and the mixture neutralised with aqueous sodium hydroxide (1M). The sticky solid formed was extracted with DCM. The organic phase was dried over sodium sulphate and concentrated in vacuo to give a solid. This was purified through silica, eluting the product with 0-12% methanol in DCM. The solid from this was triturated in diethyl ether to give the title compound, 2 g (69%) yield.