Hydroxylamine → HCID 72533800、化合物
反応式
[Cl:1][C:2]1[CH:9]=[C:8]([S:10]([CH3:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[NH2:14][OH:15]>C(O)C>[Cl:1][C:2]1[CH:9]=[C:8]([S:10]([CH3:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:3]=1[C:4](=[N:14][OH:15])[NH2:5]参加物
4
実験手順
The nitrile from Step B was dissolved into 100 mL of 1:1 ethanol/50% aqueous hydroxylamine then heated to reflux for 12 h. After evaporation of the solvent, the residue was dissolved into 400 mL of ethyl acetate then washed with saturated aqueous brine (150 mL). The organic phase was dried over magnesium sulfate, filtered, and evaporated in vacuo to yield the title compound, which was used without further purification. LC/MS 449.05 (M+1), 451.03 (M+3).
後処理
- temperaturethen heated
- temperatureto reflux for 12 h
- customAfter evaporation of the solvent
- dissolutionthe residue was dissolved into 400 mL of ethyl acetate
- washthen washed with saturated aqueous brine (150 mL)
- dry with materialThe organic phase was dried over magnesium sulfate
- filtrationfiltered
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-3d20213f5e024296a5989187f3f68b93
- 出典データセット
- uspto-grants-2010_03
- 特許番号
- US07687492B2
反応ノート
読み込み中…