tert-Butanol → HCID 86684754、化合物
反応式
C([C:4]1[CH:5]=[C:6]([F:11])[C:7]([Cl:10])=[N:8][CH:9]=1)C=C.CC[C@@H]1[C@@H]2C[C@H]([C@@H](OC3C4C(=CC=CC=4)C(O[C@@H](C4C=CN=C5C=4C=C(OC)C=C5)[C@@H]4N5C[C@H](CC)[C@@H](CC5)C4)=NN=3)C3C=CN=C4C=3C=C([O:33]C)C=C4)N(CC2)C1.[C:70]([OH:74])(C)([CH3:72])[CH3:71]>O>[Cl:10][C:7]1[N:8]=[CH:9][C:4]([CH2:71][C@@H:70]([OH:74])[CH2:72][OH:33])=[CH:5][C:6]=1[F:11]参加物
5
実験手順
To a solution of 2 (2.7 g, 16.2 mmol) in t-butanol (80 mL) and H2O (80 mL), AD-mix-beta (27.8 g) was added portion wise at 5° C. The reaction was slowly warmed to room temperature and further stirred at this temperature for 16 hrs. The reaction mixture was cooled down to 5° C. and then quenched by adding excess sodium sulfite and stirred for 20 min. The resulting mixture was diluted with water (100 mL) and extracted with ethyl acetate (100 mL×2). The organic layers were combined which was washed with brine, dried over Na2SO4, and concentrated. The obtained residue was chromatographed on silica gel eluted with hexane/ethyl acetate (20%-100%) to afford 3.2 g (98%) of 3 as a colorless oil which was slowly solidified.