Pentaerythritol → HCID 10313222, compound

Temperature

35 °C

To a solution of pentaerythritol (10.0 g) in water (600 mL) was 5% platinum/carbon (hydrous article, 13.3 g). While maintaining pH of the reaction mixture to 6˜7 by means of 8% sodium hydrogen carbonate solution, it was stirred at 35° C. for 8 hours under an atmosphere of oxygen. After catalyst was filtered, and having removed, the reaction mixture was concentrated. After having put the obtained residue through ion exchange resin Amberlyst (Amberlyst: trade name) A-21 by means of 2N hydrochloric acid, it was purified by preparative medium pressure liquid chromatography W-prep 2XY (column: main column L, inject column M; automatic condition setting: dichloromethane:methanol=4:1, Rf=0.25, preparative isolation mode GR). Furthermore, the obtained residue was purified by preparative TLC (dichloromethane:methanol=4:1) to give the title compound (123 mg) having the following physical data.

1. filtrationAfter catalyst was filtered
2. customhaving removed
3. concentrationthe reaction mixture was concentrated
4. customwas purified by preparative medium pressure liquid chromatography W-prep 2XY (column: main column L, inject column M; automatic condition setting: dichloromethane:methanol=4:1, Rf=0.25, preparative isolation mode GR)
5. customFurthermore, the obtained residue was purified by preparative TLC (dichloromethane:methanol=4:1)

ORD record

ord-bf7038bd88ff4986a16b0212524a83b9

Source dataset

uspto-grants-2011_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07968572B2