3-Methoxy-2-nitropyridine → 2-Amino-3-methoxypyridine

To a solution of 2-nitro-3-methoxypyridine (32 g, 208 mmol) in EtOAc (150 mL) and MeOH (35 mL) under a nitrogen atmosphere was added 10% palladium on carbon (1.5 g, 1.4 mmol). This mixture was purged with H2 three times and the mixture was stirred for 3 h under a hydrogen atmosphere. The reaction mixture was purged with N2 three times, filtered through Celite, and the filter cake was washed with EtOAc (2×35 ml). The combined filtrate were concentrated and dried over high vacuum to afford 25.8 grams (100%) of 2-amino-3-methoxypyridine: LCMS (m/z): 125.0 (MH+); 1H NMR (300 MHz, CDCl3): 7.66 (m, 1H), 6.90 (m, 1H), 6.61 (m, 2H), 4.64 (s, br, 2H), 3.83 (s, 3H).

1. customThis mixture was purged with H2 three times
2. customThe reaction mixture was purged with N2 three times
3. filtrationfiltered through Celite
4. washthe filter cake was washed with EtOAc (2×35 ml)
5. concentrationThe combined filtrate were concentrated
6. customdried over high vacuum

ORDレコード

ord-4978bc5377fc48e1b3f2b57e63efd495

出典データセット

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08865732B2