5,6-Dichloro-nicotinic acid tert-butyl ester synthesis
- Product Name:5,6-Dichloro-nicotinic acid tert-butyl ester
- CAS Number:1011476-27-9
- Molecular formula:C10H11Cl2NO2
- Molecular Weight:248.11
24424-99-5
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Yield:1011476-27-9 94.4%
Reaction Conditions:
with dmap in tetrahydrofuran at 50;
Steps:
3.1 Step 1 : tert-butyl 5,6-dichloropyridine-3-carboxylate
5,6-Dichloronicotinic acid (10 g, 52.08 mmol) was dissolved in 200 ml of dried THF followed by 4-dimethylaminopyridine (2 g, 24.55 mmol). The solution was treated with Boc anhydride (14.2 g, 65. 10 mmol) at r.t. Then the solution was heated up to 50°C until the gas evolution started. Then the bath was removed and the mixture was allowed to stir overnight. The solvent was evaporated under reduced pressure, the residue was dissolved in diethyl ether, washed with 1 N HCI, then with 5% water solution of ammonia and finally with water. The organic phase was dried and concentrated affording an oil (12.2 g, 94.4 %). 1H-NMR (CDCI3, δ in ppm): 8.82 (d, 1 H), 8.28 (d, 1 H), 1.61 (s, 9H).
References:
WO2014/173921,2014,A1 Location in patent:Page/Page column 55; 56
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36805-97-7
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