Ammonium Chloride → (2H-[1,3]Dioxolo[4,5-b]pyridin-2-yl)methanol

Reaction under a nitrogen atmosphere. A solution of intermediate (4) (0.042 mol) in THF (48 ml) was added dropwise to LiAlH4 (1 Min THF) (0.0466 mol) and cooled with an ice-water bath. The resulting reaction mixture was stirred for one hour at room temperature. The reaction mixture was treated carefully with a 10% NH4Cl solution and it was diluted with water and ethyl acetate. The reaction mixture was filtered over Celite and the filtrate was extracted. The separated organic layer was dried, filtered and the solvent was evaporated. The residue was washed with DCM, filtered off and dried, yielding 2.78 g of (±)-1,3-dioxolo[4,5-b]pyridine-2-methanol (intermediate 5).

1. customReaction under a nitrogen atmosphere
2. temperaturecooled with an ice-water bath
3. customThe resulting reaction mixture
4. filtrationThe reaction mixture was filtered over Celite
5. extractionthe filtrate was extracted
6. customThe separated organic layer was dried
7. filtrationfiltered
8. customthe solvent was evaporated
9. washThe residue was washed with DCM
10. filtrationfiltered off
11. customdried

ORD-Eintrag

ord-52bd9af9abde4dd88619b3dcdc6bb275

Quelldatensatz

uspto-grants-2006_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07081453B2