反应详情

4.6 g of 60% NaH are added in small portions to a solution of 36 g of the above 3,4-dichloro-α-[(2-tetrahydropyranyloxy)ethyl]benzeneacetonitrile (prepared according to PREPARATION II (a)) in 100 ml of dimethylformamide. The reaction mixture is stirred for 3 hours at room temperature and cooled to 0° C. and 22.4 g of ethyl 4-bromobutyrate in 40 ml of dimethylformamide are then added. The reaction mixture is stirred for 3 hours at room temperature, poured into water and extracted with ether and the extract is washed with a saturated solution of NaCl, dried over Na2SO4 and concentrated under vacuum. The residue obtained is purified by chromatography on silica gel using toluene as the eluent to give 24 g of the expected product.

1. temperaturecooled to 0° C.
2. stirringThe reaction mixture is stirred for 3 hours at room temperature
3. extractionextracted with ether
4. washthe extract is washed with a saturated solution of NaCl
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under vacuum
7. customThe residue obtained
8. customis purified by chromatography on silica gel