1-Bromoheptane → HCID 21849425, compound

Magnesium pieces (6.56 g) were added to anhydrous tetrahydrofuran (10 ml) in a stream of nitrogen and the mixture was stirred at room temperature. A solution (200 ml) of 1-bromoheptane (48.4 g) in anhydrous tetrahydrofuran was dropwise added thereto while heating gradually and the mixture was stirred at 40° C. for 1 hour. Thereto was dropwise added a solution (100 ml) of 2-bromobenzaldehyde (25 g) in anhydrous tetrahydrofuran at room temperature and the mixture was stirred for 1 hour. The reaction mixture was poured into a saturated, aqueous ammonium chloride solution and extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was distilled away and the residue was purified by silica gel column chromatography (eluent; ethyl acetate:hexane=1:8) to give the subject compound (18.9 g) as an oily substance.

1. temperaturewhile heating gradually
2. stirringthe mixture was stirred at 40° C. for 1 hour
3. stirringthe mixture was stirred for 1 hour
4. extractionextracted with ethyl acetate
5. washThe ethyl acetate layer was washed with saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationThe solvent was distilled away
8. customthe residue was purified by silica gel column chromatography (eluent; ethyl acetate:hexane=1:8)

ORD record

ord-3bb11544cdf24b1fbfca70941eecc65c

Source dataset

uspto-grants-1998_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05719176