Carbamic acid, (1,2-dihydro-2-oxo-3-pyridinyl)-, 1,1-dimethylethyl ester (9CI) synthesis
- Product Name:Carbamic acid, (1,2-dihydro-2-oxo-3-pyridinyl)-, 1,1-dimethylethyl ester (9CI)
- CAS Number:197229-63-3
- Molecular formula:C10H14N2O3
- Molecular Weight:210.23
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Yield:197229-63-3 99.52%
Reaction Conditions:
in tetrahydrofuran at 25 - 70; for 16 h;
Steps:
3 Compound 15
To a solution of Compound 14 (10 g, 90.82 mmol, 1 eq) in THF (150 mL) was added BOC2O (19.82 g, 90.81 mmol, 20.86 mL, 1 eq) at 25 °C. The mixture was stirred at 70 °C for 4 hrs. Then BOC2O (15.86 g, 72.65 mmol, 16.69 mL, 0.8 eq) was added and the mixture was refluxed at 70 °C for 12 hrs. TLC (Petroleum ether: Ethyl acetate = 1 : 1, Rf = 0.39) showed a new spot was formed and the reaction was completed. The reaction mixture was partitioned between H2O (300 mL) and EtOAc (180 mL). The organic phase was separated, washed with brine 120 mL (40 mLx 3), dried over Na2SO4, filtered and the filtrate was concentrated under reduced pressure to give a residue. The residue was purified by column chromatography (SiCb, Petroleum ether/Ethyl acetate=l/O to 0/1).
References:
WO2022/66776,2022,A1 Location in patent:Paragraph 0098
24424-99-5
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197229-63-3
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6332-56-5
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197229-63-3
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33630-99-8
201 suppliers
$8.00/1g
24424-99-5
820 suppliers
$13.50/25G
197229-63-3
30 suppliers
inquiry