Hexane → HCID 15238025, compound

To a solution of carbon tetrabromide (19.5 g) in methylene chloride (50 ml) was added triphenylphosphine (30.8 g) at 0° C., and the mixture was stirred for 10 min. To the mixture was added a solution of 2-formylmethyl-5-methoxy-1,2,3,4-tetrahydronaphthalene (4.09 g; the compound prepared by method described in the specification of the Japanese Patent Application No. 3-130467) in methylene chloride (25 ml) at 0° C. The mixture was stirred for 30 min at 0° C. To the mixture was gradually added n-hexane, and filtrated to remove triphenylphosphineoxide. The filtrate was washed with water and a saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate, and evaporated. The residue was purified by silica gel column chromatography (n-hexane: ethyl acetate=24:1) to give the title compound (6.42 g) having the following physical data.

1. customat 0° C
2. stirringThe mixture was stirred for 30 min at 0° C
3. filtrationfiltrated
4. customto remove triphenylphosphineoxide
5. washThe filtrate was washed with water
6. dry with materiala saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate
7. customevaporated
8. customThe residue was purified by silica gel column chromatography (n-hexane: ethyl acetate=24:1)

ORD record

ord-9d29adf1146a4475b98e00358b1621e4

Source dataset

uspto-grants-1999_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05962439