2-Amino-2-methyl-1-propanol → HCID 10847919、化合物
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([N+:11]([O-])=O)[CH:3]=1.N[C:15]([CH3:19])([CH3:18])[CH2:16][OH:17]>CCO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([NH:11][C:15]([CH3:19])([CH3:18])[CH2:16][OH:17])[CH:3]=1参加物
4
実験手順
A mixture of 20 g of 4-chloro-1,2-dinitrobenzene and 36 g of 2-amino-2-methylpropan-1-ol in 100 ml of EtOH is refluxed for 36 hours. The reaction mixture is evaporated under vacuum, the residue is extracted with AcOEt, washed with a 1N solution of HCl and with water and dried over Na2SO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica using DCM as the eluent to give 16 g of the expected product, which is used as such in the next step.
後処理
- temperatureis refluxed for 36 hours
- customThe reaction mixture is evaporated under vacuum
- extractionthe residue is extracted with AcOEt
- washwashed with a 1N solution of HCl and with water
- dry with materialdried over Na2SO4
- customthe solvent is evaporated off under vacuum
- customThe residue is chromatographed on silica
出典と根拠
- ORDレコード
- ord-24cb384b05ac4e118874adb5b78e39e0
- 出典データセット
- uspto-grants-1996_12
- 特許番号
- US05585394
反応ノート
読み込み中…