Hydrochloric Acid → 3-(Morpholin-4-yl)aniline
反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:8]=[C:9]([NH:13]C(=O)OC(C)(C)C)[CH:10]=[CH:11][CH:12]=2)[CH2:3][CH2:2]1.Cl>>[O:1]1[CH2:2][CH2:3][N:4]([C:7]2[CH:8]=[C:9]([CH:10]=[CH:11][CH:12]=2)[NH2:13])[CH2:5][CH2:6]1参加物
3
実験手順
A solution of tert-butyl (3-morpholinophenyl)carbamate (5.91 g, 21.20 mmol) in a solution of HCl (106 mL, 106.0 mmol, 1 M in MeOH) was stirred at rt overnight, then concentrated in vacuo. The residue was dissolved in water (100 mL). The soltution was basified with saturated Na2CO3 aqueous solution and extracted with CH2Cl2 (100 mL×3). The combined organic phases were washed with brine (150 mL), dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound as a light brown solid (3.42 g, 91%).
後処理
- concentrationconcentrated in vacuo
- dissolutionThe residue was dissolved in water (100 mL)
- extractionextracted with CH2Cl2 (100 mL×3)
- washThe combined organic phases were washed with brine (150 mL)
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-ae6ec9c3bee54ec0aec43474a3191766
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434695B2
反応ノート
読み込み中…