反応式
[CH3:1][N:2]([CH2:4][C:5]1[O:9][C:8]([CH2:10][S:11][CH2:12][CH2:13][NH:14][C:15]([NH:20][CH3:21])=[CH:16][N+:17]([O-:19])=[O:18])=[CH:7][CH:6]=1)[CH3:3].[ClH:22]>C(O)CC>[CH3:21][NH:20][C:15]([NH:14][CH2:13][CH2:12][S:11][CH2:10][C:8]1[O:9][C:5]([CH2:4][N:2]([CH3:1])[CH3:3])=[CH:6][CH:7]=1)=[CH:16][N+:17]([O-:19])=[O:18].[ClH:22]参加物
4
実験手順
N-[2-[[[5-(Dimethylamino)methyl-2-furanyl]methyl]thio]ethyl]-N'-methyl-2-nitro-1,1-ethenediamine (5 g) was dissolved in n-propanol (20 ml). A further quantity of n-propanol (20 ml) containing molar equivalent of hydrogen chloride was added slowly to the solution. The solution was seeded with Form 1 crystals at this temperature to induce crystallization. It was stirred further for 1-2 hrs. The hydrochloride crystallized during this period, and was filtered off. The product was washed with n-propanol (2×5 ml) and was dried at 45° C. under vacuum to give Form 1 ranitidine hydrochloride (4.49 g), m.p. 136°-137° C., purity=99.6% (HPLC).
後処理
- additionwas added slowly to the solution
- customcrystallization
- customThe hydrochloride crystallized during this period
- filtrationwas filtered off
- washThe product was washed with n-propanol (2×5 ml)
- customwas dried at 45° C. under vacuum
出典と根拠
- ORDレコード
- ord-b71a0c91fa6e49fa944dc1a130dca624
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05621120
関連ノート
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