2,6-Dihydroxy-4,5-dimethyl-nicotinonitrile synthesis
- Product Name:2,6-Dihydroxy-4,5-dimethyl-nicotinonitrile
- CAS Number:56704-29-1
- Molecular formula:C8H8N2O2
- Molecular Weight:164.16
Yield:56704-29-1 94%
Reaction Conditions:
with potassium hydroxide in methanol; for 4 h;Reflux;
Steps:
2,6-Dihydroxy-4,5-dimethylnicotinonitrile
To a slurry of ethyl 2-methyl-3-oxobutanoate (10 g, 69.4 mmol, 1 equiv) and 2-cyanoacetamide (5.8 g, 69.4 mmol, 1 equiv) was slowly added a solution of KOH (4.9 g, 87 mmol, 1.25 equiv) in MeOH (35 mL).
Stir for 1 h during which time solution became homogenous yellow before developing a cream colored precipitate.
Heat at reflux for 3 h.
Upon cooling to ambient temperature, concentrated HCl (9 mL) was added.
The off white solid was filtered and washed with ether to provide the product (10.7 g, 94%) as a cream colored solid. 1H NMR (500 MHz, DMSO-d6) δ 2.22 (s, 3H), 1.90 (s, 3H); LCMS (ESI, M+1): 165.05.
References:
US2015/232480,2015,A1 Location in patent:Paragraph 0236
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