1,2-Dichloroethane → 2-Amino-3,5-dimethylbenzamide
反応式
[NH2:1][C:2]1[C:10]([CH3:11])=[CH:9][C:8]([CH3:12])=[CH:7][C:3]=1[C:4](O)=[O:5].C1C=CC2N(O)N=[N:19]C=2C=1.C(Cl)CCl.CN>C(Cl)Cl>[NH2:1][C:2]1[C:10]([CH3:11])=[CH:9][C:8]([CH3:12])=[CH:7][C:3]=1[C:4]([NH2:19])=[O:5]参加物
6
実験手順
A solution of 2-amino-3,5-dimethyl-benzoic acid (550 mg) in DCM (30 mL) was treated with HOBt (225 mg), EDC (1280 mg), and CH3NH2 (8.5 mL, 2N in THF). The reaction mixture was stirred for 16 hours in a sealed bottle, diluted with DCM (100 mL), and washed with brine three times. The organic layer was dried (sodium sulfate), and concentrated in vacuo. The residue was purified by silica gel chromatography to provide 573 mg of 2-amino-3,5-dimethyl-benzamide: 1H NMR (300 MHz, CDCl3) δ 7.9 (s, 1H), 7.8 (s, 1H), 6.1 (bs, 1H), 5.3 (bs, 2H), 2.9 (d, 3H), 2.2 (s, 3H), 2.1 (s, 3H).
後処理
- washwashed with brine three times
- dry with materialThe organic layer was dried (sodium sulfate)
- concentrationconcentrated in vacuo
- customThe residue was purified by silica gel chromatography
出典と根拠
- ORDレコード
- ord-d547ccbcedd245069225dea4c71958f3
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08552186B2
反応ノート
読み込み中…