Hydrochloric Acid → ((3-Trifluoromethyl)phenyl)methyl-phosphonic acid
反応式
[F:1][C:2]([F:19])([F:18])[C:3]1[CH:4]=[C:5]([CH:15]=[CH:16][CH:17]=1)[CH2:6][P:7](=[O:14])([O:11]CC)[O:8]CC.Cl>CCO>[F:18][C:2]([F:1])([F:19])[C:3]1[CH:4]=[C:5]([CH:15]=[CH:16][CH:17]=1)[CH2:6][P:7](=[O:8])([OH:11])[OH:14]参加物
4
実験手順
Diethyl 3-trifluoromethylbenzylphosphonate (3.0 g, 10.0 mmol) was dissolved in a mixture; of 50 mL of conc hydrochloric acid and 1.5 mL of EtOH and was heated at reflux for 17 hours. After cooling the clear reaction mixture in an ice-water mixture, the white crystalline solid which formed was collected to give 2.05 g (84.3%) of the analytical product, mp=163°-164° C. 300 MHz 1H NMR (DMSO-D6) δ, 7.40-7.75 (m, 4H, aromatic), 3.09 (d, 2H, J=21.5 Hz, PCH2). D.C.I.M.S.[MH+, 241].
後処理
- temperatureat reflux for 17 hours
- customthe white crystalline solid which formed
- customwas collected
出典と根拠
- ORDレコード
- ord-b557fdc824884b9a8fe9abeb0754611e
- 出典データセット
- uspto-grants-1996_07
- 特許番号
- US05532226
反応ノート
読み込み中…