Hydroxylamine → tert-butyl 4-(N-hydroxyamidino)-piperazine-1-carboxylate
反応式
[C:1]([N:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:5][CH2:4]1)#[N:2].[NH2:16][OH:17]>C(O)C>[OH:17][NH:16][C:1](=[NH:2])[N:3]1[CH2:4][CH2:5][N:6]([C:9]([O:11][C:12]([CH3:14])([CH3:13])[CH3:15])=[O:10])[CH2:7][CH2:8]1参加物
4
実験手順
To a solution of tert-butyl 4-cyanopiperazine-1-carboxylate (15 g, 76 mmol) in ethanol (150 mL) was added hydroxylamine (50% aqueous solution, 6.2 mL, 92 mmol) and the reaction mixture was stirred at RT for 6 hours. The solvent was evaporated under vacuum and the solid obtained was triturated with hexane (100 mL) and filtered to obtain 15 g (80%) of the title compound as a solid. TLC-Chloroform/methanol (9/1): Rf=0.15.
後処理
- customThe solvent was evaporated under vacuum
- customthe solid obtained
- customwas triturated with hexane (100 mL)
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-ec7ddd5bec6f4099bb5f3dc07cecc918
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08247437B2
反応ノート
読み込み中…