Formaldehyde → HCID 68675855, 화합물
반응식
[ClH:1].[CH:2]1([C@H:8]2[N:13]3[CH:14]=[C:15]([C:20]([N:22]4[CH2:27][C@H:26]([CH3:28])[NH:25][C@H:24]([CH3:29])[CH2:23]4)=[O:21])[C:16]4[CH:17]=[CH:18][CH:19]=[C:11]([C:12]=43)[O:10][CH2:9]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.C=O.[C:32](O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>C(O)C>[ClH:1].[CH:2]1([C@H:8]2[N:13]3[CH:14]=[C:15]([C:20]([N:22]4[CH2:23][C@H:24]([CH3:29])[N:25]([CH3:32])[C@H:26]([CH3:28])[CH2:27]4)=[O:21])[C:16]4[CH:17]=[CH:18][CH:19]=[C:11]([C:12]=43)[O:10][CH2:9]2)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]1참가 물질
5
실험 절차
To a solution of (R)-3-cyclohexyl-2,3-dihydro-6-[(cis)-3,5-dimethylpiperazin-1-yl-carbonyl]pyrrolo[1,2,3-de]-1,4-benzoxazine hydrochloride salt (100 mg, 0.26 mmol) in ethanol (10 ml) was added formaldehyde (37% in water; 1 ml, 12.5 mmol) and sodium triacetoxyborohydride (200 mg, 0.93 mmol). The mixture was stirred at room temperature for 30 minutes. The solvent was removed in vacuo. The residue was purified by flash chromatography eluting with 1-10% (v/v) methanol in dichloro-methane to afford the title compound as the free base. Hydrochloride salt formation was achieved by the addition of hydrogen chloride (2 M solution in diethyl ether; 2 ml) to the free base in dichloromethane (1 ml). The precipitate was filtered and dried to afford the title compound (1:1 hydrochloride salt). EsIMS: m/z=396.1 [M+H]+, 268; [α]D22−19.6° (c=2.1 mg/ml in methanol).