Water → 2-amino-N-ethylbenzamide
反応式
[C:1]12[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=1)[NH:6]C(=O)[O:4][C:2]2=O.O.[CH2:14]([NH2:16])[CH3:15]>CO>[NH2:6][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:1]=1[C:2]([NH:16][CH2:14][CH3:15])=[O:4]参加物
5
実験手順
A round-bottomed flask was charged with isatoic anhydride (5.0 g, 0.030 mol), 200 mL water, and 5 mL of methanol. Ethylamine (2N in methanol, 18.4 mL, 0.036 mol) was added slowly to the reaction mixture. After 1 h, the reaction mixture was concentrated to 20 mL. The reaction mixture was acidified with 1N HCl and extracted with EtOAc. The aqueous layer was basified with 6N NaOH and extracted with EtOAc. The EtOAc layer was dried over Na2SO4, filtered, and concentrated to dryness to afford 2-amino-N-ethylbenzamide (4.6 g, 91%): Mass (M+H)+=165.
後処理
- concentrationthe reaction mixture was concentrated to 20 mL
- extractionextracted with EtOAc
- extractionextracted with EtOAc
- dry with materialThe EtOAc layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated to dryness
出典と根拠
- ORDレコード
- ord-09bf447510844201a6e873b57c4cd7e1
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07884098B2
反応ノート
読み込み中…