tert-butyl 2-carbamothioylpiperidine-1-carboxylate synthesis
- Product Name:tert-butyl 2-carbamothioylpiperidine-1-carboxylate
- CAS Number:569348-09-0
- Molecular formula:C11H20N2O2S
- Molecular Weight:244.35
388077-74-5
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Yield:569348-09-0 330 mg
Reaction Conditions:
with Lawessons reagent in toluene at 80; for 16 h;Inert atmosphere;
Steps:
tert-butyl 2-carbamothioylpiperidine-l-carboxylate (3)
To a solution of tert-butyl 2- carbamoylpiperidine-l-carboxylate 2 (2.0 g, 8.77 mmol) in dry toluene (20 mL) was added Lawesson's reagent (2.13 g, 5.26 mmol) at N2 atmosphere. The resulting solution was stirred at 80°C for 16 h. The mixture was diluted with ethyl acetate (30 mL), and washed with saturated aqueous (sat. aq.) Na2C03 (2 x 20 mL) and brine (2 x 20 mL). The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated to give crude product which was purified by silica gel column chromatography eluting with 4 : 1 PE/EA to get the title compound (330 mg, 15%) as white solid. MS (ESI): m/z = 245.2 [M + H]+.
References:
WO2015/48662,2015,A2 Location in patent:Page/Page column 89
41115-30-4
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98303-20-9
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