Ammonia → 3-Amino-2-chlorobenzamide
反応式
[NH2:1][C:2]1[C:3]([Cl:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5](O)=[O:6].CC[N:14](C(C)C)C(C)C.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.N>C(Cl)Cl.O.CCOC(C)=O>[NH2:1][C:2]1[C:3]([Cl:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([NH2:14])=[O:6]参加物
9
実験手順
To a solution of 3-amino-2-chlorobenzoic acid (5.8 mmol) in 12 mL DCM were added 3.0 mL DIPEA, HOBT (7.0 mmol) and EDC.HCl (7.0 mmol) followed by the addition of 0.67 mL of a solution of NH3 in water (13M). The mixture was stirred at RT overnight, EtOAc was then added and the mixture was extracted with water, sat. aq. NaHCO3 solution and brine. The organic layer was dried over MgSO4 and concentrated in vacuo to obtain the desired compound as yellow solid.
後処理
- extractionthe mixture was extracted with water, sat. aq. NaHCO3 solution and brine
- dry with materialThe organic layer was dried over MgSO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-94310c0c15f946ef87d7511c86cc4499
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09221832B2
反応ノート
読み込み中…
