5-Fluoro-6-nitro-2,3-dihydro-1,3-benzoxazol-2-one → 6-Amino-5-fluoro-2,3-dihydro-1,3-benzoxazol-2-one
反応式
[F:1][C:2]1[C:3]([N+:12]([O-])=O)=[CH:4][C:5]2[O:9][C:8](=[O:10])[NH:7][C:6]=2[CH:11]=1>O1CCCC1.[C].[Pd]>[NH2:12][C:3]1[C:2]([F:1])=[CH:11][C:6]2[NH:7][C:8](=[O:10])[O:9][C:5]=2[CH:4]=1参加物
4
実験手順
To a solution of 5-fluoro-6-nitro-2(3H)-benzoxazolone (20 g, 0.1 mole) in 300 ml tetrahydrofuran was added 2 g palladium carbon (5%) under nitrogen atmosphere. The mixture was hydrogenated with a Parr shaker for 10 hours at 45 psi. The precipitate which resulted from hydrogenation was redissolved by adding tetrahydrofuran. The catalyst was removed by filtration and the filtrate was concentrated to give 18.1 g of the title compound as a brown solid: m.p. 180°-182° C. (dec.).
後処理
- customThe precipitate which resulted from hydrogenation
- dissolutionwas redissolved
- customThe catalyst was removed by filtration
- concentrationthe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-8c23a550a38c457c85ee5b7ec5c093fb
- 出典データセット
- uspto-grants-1992_09
- 特許番号
- US05149821
反応ノート
読み込み中…