Quinone → HCID 20089837、化合物
反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[CH:5][C:6](=[O:9])O[CH:8]=1.C1(=O)[CH:17]=[CH:16][C:15](=[O:18])[CH:14]=[CH:13]1>ClC1C=CC=CC=1Cl>[F:10][C:2]([F:1])([F:11])[C:3]1[CH:4]=[C:5]2[C:14](=[CH:13][CH:8]=1)[C:15](=[O:18])[CH:16]=[CH:17][C:6]2=[O:9]参加物
4
実験手順
A mixture of 1.64 g (0.01 mmol) of 5-trifluoromethyl-2-oxo-2H-pyrane and 5.4 g (0.05 mol) of 1,4-benzoquinone in 7 ml of 1,2-dichlorobenzene is heated for 12 hours to 180° C. The reaction mixture is then concentrated by evaporation at 90°/20 mbar, and the distillation residue is chromatographed over 150 g of silica gel 60 (eluant: 19:1 mixture of CH2Cl2 /acetone; 0.3 bar overpressure). Yield: 1.82 g (80.52%); m.p. 80°-85° C.
後処理
- temperatureis heated for 12 hours to 180° C
- concentrationThe reaction mixture is then concentrated by evaporation at 90°/20 mbar
- distillationthe distillation residue is chromatographed over 150 g of silica gel 60 (eluant: 19:1 mixture of CH2Cl2 /acetone; 0.3 bar overpressure)
出典と根拠
- ORDレコード
- ord-03fefac708754589a854650a52794283
- 出典データセット
- uspto-grants-1990_07
- 特許番号
- US04940516
反応ノート
読み込み中…