Ethanol → (5-Amino-2-chlorophenyl)(phenyl)methanone

HRID 392440

反応式

HRID 392440 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].[Sn](Cl)Cl.C(O)C.C([O-])(O)=O.[Na+]>CCOC(C)=O>[NH2:16][C:13]1[CH:14]=[CH:15][C:2]([Cl:1])=[C:3]([CH:12]=1)[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5]

参加物

6

反応条件

温度
70 °C

実験手順

2-Chloro-5-nitrobenzophenone (1.3 g,5.0 mmol), tin(II) chloride (4.5 g, 20 mmol), and ethanol (20 ml) were mixed and heated at 70° C. for 1 h. After cooling to room temperature, to the reaction mixture were added ice, EtOAc and aqueous NaHCO3 and it was stirred for 30 min. The organic layer was washed with brine and dried over MgSO4. Filtration and evaporation afforded 5-amino-2-Chlorobenzophenone. 1H NMR, 7.85(m,2H), 7.30-7.66 (m,3H7.20 (d,1H,J=8.8 Hz), 6.60-6.80 (m,2H). MS calcd 231.1; MS (M+1) 232.0.

後処理

  1. temperatureAfter cooling to room temperature, to the reaction mixture
  2. washThe organic layer was washed with brine
  3. dry with materialdried over MgSO4
  4. filtrationFiltration and evaporation

出典と根拠

ORDレコード
ord-e1b29d11510c40008c7c6efbe6135613
出典データセット
uspto-grants-2004_10
特許番号
US06800651B2

関連ノート

読み込み中…