1-tert-Butoxycarbonylpiperidine-4-carboxylic acidmethyl amide synthesis
- Product Name:1-tert-Butoxycarbonylpiperidine-4-carboxylic acidmethyl amide
- CAS Number:544696-01-7
- Molecular formula:C12H22N2O3
- Molecular Weight:242.31
84358-13-4
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544696-01-7
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Yield:544696-01-7 92%
Reaction Conditions:
Stage #1: N-[(tert-butoxy)carbonyl]piperidine-4-carboxylic acidwith O-(benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate;triethylamine in tetrahydrofuran at 20; for 1 h;
Stage #2: methylaminewith triethylamine in tetrahydrofuran; for 48 h;
Steps:
II.4.a
ll.4.a4-Methylcarbamoyl-piperidine-1-carboxylic acid te/f-butyl esterTo a solution of 6 g (26,17 mmol) piperidine-1 ,4-dicarboxylic acid mono-te/f-butyl ester in 30 ml of dry THF are added 8,477 g (26,4 mmol) of TBTU and 3,7 ml (26,4 mmol) of triethylamine. The reaction mixture is stirred at room temperature for one hour. 3,7 ml (26,4 mmol) of triethylamine and 13,5 ml (26,4 mmol) of methylamine solution (2M) are added. The reaction mixture is stirred for 48 hours, diluted with water and extracted with EtOAc. The organic phase is dried over sodium sulphate.Yield: 5.8 g (92% of theory),EII Mass spectrum: m/z = 243 [M+H]+
References:
WO2008/71646,2008,A1 Location in patent:Page/Page column 80
74-89-5
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$13.44/25ML
544696-01-7
32 suppliers
$12.00/250mg
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84358-13-4
341 suppliers
$5.00/5g
544696-01-7
32 suppliers
$12.00/250mg