2,6-Pyridinedimethanol → 2,6-Diformylpyridine

This preparation procedure followed the literature procedure (J. Chem. Soc., Dalton Trans. 1984-1937). To the mixture of 11.51 g of 2,6-pyridine-dimethanol (8.28 mmol) and 9.99 g of SeO2, was added 200 mL of 1,4-dioxane. The mixture was then refluxed for 4 h and filtered. The filtrate was concentrated under reduced pressure. The solid was dissolved in CH2Cl2 and passed through a silica gel plug. The solution was concentrated, and the solid was recrystallized from 60 mL of acetone and 100 mL of hexanes to afford 9.6 g of white crystal (71%), which was kept under N2. 1H NMR (CDCl3) δ 8.02-8.12 (m, 3H), 10.08 (s, 2H), 13C NMR δ 125.7, 138.8, 153.3, 192.7.

1. customThis preparation procedure
2. temperatureThe mixture was then refluxed for 4 h
3. filtrationfiltered
4. concentrationThe filtrate was concentrated under reduced pressure
5. dissolutionThe solid was dissolved in CH2Cl2
6. concentrationThe solution was concentrated
7. customthe solid was recrystallized from 60 mL of acetone and 100 mL of hexanes

ORD-Eintrag

ord-0360aa58883b4023a40e4b88e037091d

Quelldatensatz

uspto-grants-2002_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06380392B1