Methanol → (4,5-Difluoro-2-nitrophenyl)methanol

To a solution of to 4,5-difluoro-2-nitrobenzoic acid (25.9 g) in THF (90 ml), cooled to 0° C., was carefully added borane-tetrahydrofuran complex (319 ml, 1M in THF). After the addition was complete, the mixture was stirred at 60° C. for 3 h. Methanol (150 ml) was added to the mixture at 0° C. and after 10 minutes the mixture was concentrated in vacuo. The residue was poured into water and extracted with ethyl acetate. The organic layer was washed with sat. aq. NaCl, dried (MgSO4), filtered and concentrated in vacuo.

1. additionAfter the addition
2. concentrationwas concentrated in vacuo
3. additionThe residue was poured into water
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with sat. aq. NaCl
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo

ORD-Eintrag

ord-3154be931743426e9e0a4e705f9b1e44

Quelldatensatz

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08022218B2