N-Boc-4-MethylpiperidinecarbothioaMide synthesis
- Product Name:N-Boc-4-MethylpiperidinecarbothioaMide
- CAS Number:951745-01-0
- Molecular formula:C12H22N2O2S
- Molecular Weight:258.38
343788-67-0
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Yield:951745-01-0 36%
Reaction Conditions:
with Lawessons reagent in 1,4-dioxane at 20; for 15 h;
Steps:
136
To a solution of 1-tert-butoxycarbonyl-4-methylpiperidine-4-carboxamide (Reference Example 135) (277 mg, 1.14 mmol) in 1,4-dioxane (10 ml) was added a Lawesson's reagent (257 mg, 0.635 mmol), and the mixture was stirred at room temperature for 15 hours. The reaction solution was concentrated under a reduced pressure, and the residue was purified by flash chromatography (silica gel, n-hexane/ethyl acetate) to give a title compound (107 mg, 0.414 mmol, 36%) as a white solid. 1H-NMR (400 MHz, CDCl3) δ: 1.35 (3H, s), 1.45 (9H, s), 1.59-1.69 (2H, m), 2.06-2.21 (2H, m), 3.45-3.48 (4H, m), 6.99 (1H, brs), 7.63 (1H, brs).
References:
EP2009006,2008,A1 Location in patent:Page/Page column 90
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