Methyl iodide → HCID 58822115, compound

Temperature

0 °C

The product (4.63 g) obtained by the reaction in 2) was dissolved in tetrahydrofuran (50 ml), potassium bis(trimethylsilyl)amide (0.5N toluene solution, 80 ml) was added, and methyl iodide (2.93 ml) was then added. After heating the mixture to 0° C., it was stirred for 1 hour, quenched with a saturated aqueous solution of ammonium chloride and then diluted with diethyl ether. An organic layer was separated, washed with saturated saline and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:4) to obtain the title compound (3.7 g) as a colorless oil.

1. customquenched with a saturated aqueous solution of ammonium chloride
2. additiondiluted with diethyl ether
3. customAn organic layer was separated
4. washwashed with saturated saline
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off under reduced pressure
7. customthe residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:4)

ORD record

ord-65da56d9406846b882efbe99f9bd98a2

Source dataset

uspto-grants-2011_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07935824B2