5-Fluoroindanone oxime → 5-Fluoro-2,3-dihydro-1H-inden-1-amine
反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[N:11]O)[CH2:6][CH2:5]2>C(O)(=O)C.[Zn]>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[CH:7]([NH2:11])[CH2:6][CH2:5]2参加物
4
実験手順
Zinc powder (20.2 g) was added during three hours to the stirred solution of the above oxime (20.2 g) in acetic acid (200 ml) which maintains the temperature at 25°-35° C. The resulting mixture was stirred an additional 12 hours at room temperature. The solids were removed by filtration and the filtrate concentrated in vacuo. The concentrated filtrate was partitioned between water and toluene and the aqueous phase adjusted to pH 12 with ammonium hydroxide and extracted with toluene. Solvent removal in vacuo gave 5-fluoro-1-aminoindan (17.8 g) as a colored oil.
後処理
- customat 25°-35° C
- customThe solids were removed by filtration
- concentrationthe filtrate concentrated in vacuo
- customThe concentrated filtrate was partitioned between water and toluene
- extractionextracted with toluene
- customSolvent removal in vacuo
出典と根拠
- ORDレコード
- ord-308f788b92cc49588ca4ad24af84b0b0
- 出典データセット
- uspto-grants-1996_01
- 特許番号
- US05486541
反応ノート
読み込み中…