Ethyl Acetate → HCID 12523650, compound

All batches of the material were combined, loaded in dichloromethane and purified on silica (100 g) using a 0-25% gradient of ethyl acetate-cyclohexane over 40 mins using a Flashmaster II. The appropriate fractions were combined and evaporated in vacuo, a solution of the residue (3.42 g, 14.9 mmol) and 10% palladium on carbon (684 mg) in ethyl acetate (100 ml) was hydrogenated at atmospheric pressure and room temperature for 24 hours. The catalyst was filtered through Celite and the filtrate concentrated in vacuo to give the title compound as a yellow oil (2.22 g).

1. custompurified on silica (100 g)
2. customover 40 mins
3. customevaporated in vacuo
4. filtrationThe catalyst was filtered through Celite
5. concentrationthe filtrate concentrated in vacuo

ORD record

ord-ef244b934398431c94eeaaa38faf87c8

Source dataset

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07977344B2