Sulfuric Acid → HCID 14814852、化合物
反応式
N[C:2]1[C:3]([CH3:13])=[CH:4][C:5]([CH3:12])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8].[OH:14]S(O)(=O)=O.N([O-])=O.[Na+]>O>[OH:14][C:2]1[C:3]([CH3:13])=[CH:4][C:5]([CH3:12])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8]参加物
5
実験手順
Methyl 5-amino-2,4-dimethylbenzoate (0.752 g, 4.20 mmol) in 5 mL water was cooled with an ice bath. H2SO4 (1.1 mL, 21 mmol) was added followed by a solution of sodium nitrite (0.301 g, 4.4 mmol) in 3 mL of water. The reaction was stirred in an ice bath for 30 min, and then in a 100° C. oil bath for 60 min. The reaction was cooled to rt and partitioned between EtOAc and brine. The organic phase was dried (Na2SO4) and concentrated to give the title compound as a yellow oil. 1H NMR (CDCl3) δ 7.48 (s, 1H), 7.00 (s, 1H), 5.95 (bs, 1H), 3.90 (s, 3H), 2.50 (s, 3H), 2.28 (s, 3H).
後処理
- waitin a 100° C. oil bath for 60 min
- custompartitioned between EtOAc and brine
- dry with materialThe organic phase was dried (Na2SO4)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-fe4d7a7ce46d4a9480adc6f27919bf13
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08410284B2
反応ノート
読み込み中…