3-methylazetidine-1-sulfonamide synthesis
- Product Name:3-methylazetidine-1-sulfonamide
- CAS Number:1418112-83-0
- Molecular formula:C4H10N2O2S
- Molecular Weight:150.2
1418112-84-1
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1418112-83-0
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Yield:1418112-83-0 60.3 g
Reaction Conditions:
with palladium 10% on activated carbon;hydrogen in ethanol; under 2250.23 Torr; for 16 h;
Steps:
B.ii ii) 3-Methylazetidine-l-sulfonamide
The sub-title product of step (i) (132 g) split into 2 reactors was added to a stirred solution of 10% Pd/C (4.94 g) in ethanol (1000 mL). The mixture was hydrogenated at 3.00 bar for 16 hours. The solvent was evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution 30% ethyl acetate in dichloromethane (stained with KMn04). Pure fractions were evaporated to dryness to afford the title product (60.3 g) as a white solid. 1H NMR (500 MHz, CDC13) δ 6.82 (s, 2H), 3.75 (t, J = 8.0 Hz, 2H), 3.36 - 3.24 (m, 2H), 2.59 - 2.46 (m, 1H), 1.13 (d, J = 6.8 Hz, 3H).
References:
WO2013/8002,2013,A1 Location in patent:Page/Page column 48