反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])=[CH:4][CH:3]=1.C([Li:21])CCC>C1C=CC=CC=1.CCCCCC>[CH2:9]([O:8][C:5]1[CH:6]=[CH:7][C:2]([Li:21])=[CH:3][CH:4]=1)[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]参加物
実験手順
31.38 g (110.0 mmol) of 1-bromo-4-octyloxybenzene in 80 ml of benzene and 81 ml (130.0 mmol) of a 1.6-molar n-butyllithium solution in hexane are stirred at room temperature under argon for 4 hours. The 4-octyloxyphenyllithium formed as a white precipitate is filtered off under argon, washed twice with 20 ml of n-hexane, dried in vacuo and slowly added dropwise as a solution in 60 ml of tetrahydrofuran at 0° C. under argon to a solution of 11.51 g (100.0 mmol) of 2,6-difluoropyridine in 80 ml of tetrahydrofuran. After a reaction time of 1 hour at 0° C., sodium chloride solution is added, the mixture is taken up in ether, the organic phase is washed with sodium chloride solution, dried over sodium sulfate, filtered, the solvent is removed from the filtrate, and the residue is purified by chromatography (silica gel, 9:1 hexane/ethyl acetate), giving 4.00 g of 2-fluoro-6-(4-octyloxyphenyl)pyridine. ##STR17##
出典と根拠
- ORDレコード
- ord-e6d1a2fd748a44f1b1032e827b166bcf
- 出典データセット
- uspto-grants-1997_05
- 特許番号
- US05630962
関連ノート
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