Borane;tetrahydrofuran → HCID 178419171、化合物
反応式
[CH3:1][N:2]([CH3:24])[C:3]1[C:8]([CH3:9])=[CH:7][C:6]([PH:10](=O)[C:11]2[CH:16]=[C:15]([CH3:17])[C:14]([N:18]([CH3:20])[CH3:19])=[C:13]([CH3:21])[CH:12]=2)=[CH:5][C:4]=1[CH3:23].[BH3:25].O1CCCC1>C1(C)C=CC=CC=1>[CH3:24][N:2]([CH3:1])[C:3]1[C:8]([CH3:9])=[CH:7][C:6]([PH:10][C:11]2[CH:16]=[C:15]([CH3:17])[C:14]([N:18]([CH3:19])[CH3:20])=[C:13]([CH3:21])[CH:12]=2)=[CH:5][C:4]=1[CH3:23].[BH3:25]参加物
4
実験手順
Under an argon atmosphere, to a solution of bis(4-dimethylamino-3,5-dimethylphenyl)phosphine oxide (4.6 g, 14 mmoL) synthesized in Example 1 in toluene (30 mL) was added borane-tetrahydrofuran solution (71 mL, 5.4 equivalents) at room temperature over 2 hr. Then, silica gel (8.7 g, 10.8 equivalents) was added to the mixture, and the mixture was stirred at room temperature for 1.5 hr. The silica gel was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (silica gel 20 g, toluene) and the residue was recrystallized from n-hexane to give the title compound (3.0 g, white crystals). yield 65%.