Acetic Acid → 2-Methylfluorene
反応式
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][C:2]=1[CH:14]=O.C(O)(=O)C.[H][H]>C(OCC)(=O)C.CCCCCC.[OH-].[OH-].[Pd+2]>[CH3:14][C:2]1[CH:3]=[CH:4][C:5]2[C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[CH2:12][C:13]=2[CH:1]=1参加物
7
実験手順
A solution of 2-fluorenecarboxaldehyde (15 g, 77.1 mmol) in 250 mL of 10% solution of acetic acid in ethyl acetate was hydrogenated at 80 psi of hydrogen during 24 hours at room temperature over 20% palladium hydroxide on carbon (catalytic amount). The reaction was monitored by TLC (silica, 25% ethyl acetate in hexane). The catalyst was filtered off, evaporation of the solvents followed by recrystallization of the residual solid from ethanol:water 5:1 afforded 9.6 g (69.0%) of the product as colorless solid.
後処理
- filtrationThe catalyst was filtered off
- customevaporation of the solvents
- customfollowed by recrystallization of the residual solid from ethanol:water 5:1
出典と根拠
- ORDレコード
- ord-8f6e1c3af9924fbfa04f62eb84f9198e
- 出典データセット
- uspto-grants-1992_01
- 特許番号
- US05079260
反応ノート
読み込み中…