Methyl iodide → HCID 86750226, Verbindung

To a suspension of sodium hydride (6.1 mg) in tetrahydrofuran (1.5 ml) was added a solution of the compound prepared in example 15 (70 mg) in tetrahydrofuran (3 ml) under an atmosphere of argon. The mixture was stirred for 30 min at room temperature. To the mixture were successively added methyl iodide (261 mg) and hexamethylphosphoramide (1 ml), After stirred for 2 h at room temperature, the mixture was diluted with ethyl acetate and water. The mixture was extracted with ethyl acetate. The extract 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 (ethyl acetate:hexane =2:3) to give the title compound (27 mg) having the following physical data.

1. stirringAfter stirred for 2 h at room temperature
2. extractionThe mixture was extracted with ethyl acetate
3. washThe extract was washed with water
4. dry with materiala saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate
5. customevaporated
6. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane =2:3)

ORD-Eintrag

ord-0a40a64eb5fd4534b8890b7eadef87df

Quelldatensatz

uspto-grants-1997_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05596009