反应详情

温度

0 °C

N-chlorosuccinimid (134 mg) is added to a solution of crude 4-bromo-naphthalene-1-carbaldehyde oxime (250 mg) in DMF (3 ml). After 1 hour at 40° C., the reaction is cooled down to 0° C. and 1,3-dichloro-5-(1-trifluoromethyl-vinyl)-benzene (240 mg) and triethylamine (0.15 ml) are added. The reaction is further reacted at room temperature for 16 hours. Water is added and the reaction mixture is extracted with ethyl acetate. The organic phase is washed with a saturated aqueous solution of NaCl, dried over MgSO4 and concentrated in vacuo. The crude product is purified on a semi-preparative HPLC to yield 3-(4-bromo-naphthalen-1-yl)-5-(3,5-dichloro-phenyl)-5-trifluoromethyl-4,5-dihydro-isoxazole as colorless crystals: m.p. 127-130° C.

1. customThe reaction is further reacted at room temperature for 16 hours
2. extractionthe reaction mixture is extracted with ethyl acetate
3. washThe organic phase is washed with a saturated aqueous solution of NaCl
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe crude product is purified on a semi-preparative HPLC