Hydrochloric Acid → HCID 178491370、化合物
反応式
Cl.[CH3:2][O:3][C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH3:13])[C:5]=1[CH2:6][NH2:7].[N-:14]([C:17]#[N:18])[C:15]#[N:16].[Na+]>>[C:15]([NH:14][C:17]([NH:7][CH2:6][C:5]1[C:8]([O:12][CH3:13])=[CH:9][CH:10]=[CH:11][C:4]=1[O:3][CH3:2])=[NH:18])#[N:16]参加物
4
実験手順
15 ml 2N hydrochloric acid were added to 5.0 g (29.9 mmol) 2,6-dimethoxybenzylamine and the aqueous phase was subsequently removed under vacuum. The residue was then dissolved in 50 ml 1-butanol and 2.66 g (29.9 mmol) of sodium dicyanamide were added. The reaction mixture was heated for 5.5 hours at reflux and stirred for 12 hours at room temperature. The precipitate formed was filtered off, was washed with diethylether; 6.81 g.
後処理
- customthe aqueous phase was subsequently removed under vacuum
- dissolutionThe residue was then dissolved in 50 ml 1-butanol
- temperatureThe reaction mixture was heated for 5.5 hours
- temperatureat reflux
- customThe precipitate formed
- filtrationwas filtered off
- washwas washed with diethylether
出典と根拠
- ORDレコード
- ord-0740ffcdbd084f38a1576fed031345a4
- 出典データセット
- uspto-grants-2013_07
- 特許番号
- US08481576B2
反応ノート
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