Sodium Hydroxide → 4-Amino-2-fluoro-N-methylbenzenesulfonamide
反応式
[F:1][C:2]1[CH:3]=[C:4]([NH:13]C(=O)C)[CH:5]=[CH:6][C:7]=1[S:8](=[O:12])(=[O:11])[NH:9][CH3:10].[OH-].[Na+]>Cl>[NH2:13][C:4]1[CH:5]=[CH:6][C:7]([S:8]([NH:9][CH3:10])(=[O:12])=[O:11])=[C:2]([F:1])[CH:3]=1参加物
4
実験手順
The above prepared N-(3-fluoro-4-methylsulfamoylphenyl)acetamide (1.55 g, 6.3 mmol) was suspended in 40 mL of 6M HCl and heated to reflux for 1 hr. The reaction was cooled in an ice bath and an NaOH solution was added to adjust the mixture to pH 5. The resulting white precipitate was isolated by filtration and was washed with water and dried to yield 1.07 g (83%) of the title compound. MS (m/z, ES+): 205.0 (M+1, 100%); 1H NMR (500 MHz, ppm, DMSO-d6): 7.35 (m, 1H), 7.12 (m, 1H), 6.40 (m, 2H), 6.23 (s, 2H), 2.40 (s, 3H).
後処理
- temperatureheated
- temperatureto reflux for 1 hr
- temperatureThe reaction was cooled in an ice bath
- customThe resulting white precipitate was isolated by filtration
- washwas washed with water
- customdried
出典と根拠
- ORDレコード
- ord-119cbd4f5cba4fdc9d81423318e3a95e
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434720B2
反応ノート
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