Acetic Acid → N-[(2,5-Difluorophenyl)methylidene]hydroxylamine
反応式
[F:1][C:2]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][C:3]=1[CH:4]=O.Cl.[NH2:12][OH:13].[OH-].[Na+].C(O)(=O)C>CCO.O>[F:1][C:2]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][C:3]=1[CH:4]=[N:12][OH:13]参加物
7
実験手順
2,5-Difluorobenzaldehyde (28.5 g, 0.20 mol) was dissolved in 30 ml EtOH. 80 ml water, 80 g crushed ice and hydroxylamine hydrochloride (15.3 g, 0.22 mol) were added. 250 ml (0.50 mol) 2N NaOH were added drop wise and the yellow solution was stirred for 3 hours at room temperature. The reaction mixture was neutralized to pH 6 with acetic acid. The formed suspension was diluted with water and filtered. The crystals were washed with water and dried 2 hours at 50° C. and <20 mbar to obtain the desired product as a white solid (26.1 g, 83%). MS (m/e): 156.0 (M−H+).
後処理
- additionwere added
- filtrationfiltered
- washThe crystals were washed with water
- customdried 2 hours at 50° C.
出典と根拠
- ORDレコード
- ord-cf8be64000aa424bb5ae7f2eb474068b
- 出典データセット
- uspto-grants-2010_12
- 特許番号
- US07858630B2
反応ノート
読み込み中…