Hydrochloric Acid → HCID 22716029、化合物
反応式
[ClH:1].[NH2:2][CH2:3][C:4]1[N:8]([CH3:9])[N:7]=[C:6]([C:10]([NH2:12])=[O:11])[N:5]=1>C(OCC)(=O)C>[ClH:1].[NH2:2][CH2:3][C:4]1[N:8]([CH3:9])[N:7]=[C:6]([C:10]([NH2:12])=[O:11])[N:5]=1参加物
4
実験手順
Hydrogen chloride was passed to saturation at 5° C. to a solution of 4.7 g (not more-than 18.4 mmol) of 5-aminomethyl-1-methyl-1H-[1,2,4]-triazole-3-carboxamide in 600 ml of ethyl acetate, during which process a white precipitate formed. The mixture was stirred overnight at room temperature and concentrated on a rotary evaporator, diethyl ether was added, the mixture was concentrated and again taken up in diethyl ether, and the precipitate was filtered off and dried. This gave 3.7 g of a white solid which still contained ammonium chloride. 1H NMR (270 MHz, DMSO-d6): δ=3.95 (s, 3H), 4.3 (bs, 2H), 7.6 (bs, 1H), 7.75 (bs, 1H), 8.7-8.9 (m, 2H).
後処理
- customsaturation at 5° C.
- customduring which process a white precipitate formed
- concentrationconcentrated on a rotary evaporator, diethyl ether
- additionwas added
- concentrationthe mixture was concentrated
- filtrationthe precipitate was filtered off
- customdried
出典と根拠
- ORDレコード
- ord-f3fe6551de5947e99c3e23307ade7bd1
- 出典データセット
- uspto-grants-2004_05
- 特許番号
- US06740647B1
反応ノート
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