1-BOC-(2S)-[N-METHOXY-N-METHYLCARBAMOYL]PIPERIDINE synthesis

5synthesis methods

Product Name:1-BOC-(2S)-[N-METHOXY-N-METHYLCARBAMOYL]PIPERIDINE
CAS Number:203056-27-3
Molecular formula:C13H24N2O4
Molecular Weight:272.34

6638-79-5 Synthesis

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26250-84-0
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1-BOC-(2S)-[N-METHOXY-N-METHYLCARBAMOYL]PIPERIDINE

203056-27-3
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Yield:203056-27-3 94%

Reaction Conditions:

Stage #1: (S)-(-)-1-(tert-butoxycarbonyl)-2-piperidinecarboxylic acidwith 1,1'-carbonyldiimidazole in dichloromethane at 20;
Stage #2: N,O-dimethylhydroxylamine*hydrochloride in dichloromethane at 20; for 17 h;

Steps:

1.1 (S)-1-(tert-butoxycarbonyl)-2-(N-methyl-N-methoxy)-carbamoylpiperidine 2:

Dissolve 20.0g (87.2mmol) (S)-1-(tert-butoxycarbonyl)-2-piperidinecarboxylic acid 1 in 400mL dichloromethane,slowly add 18.4g (113.5 mmol) N,N’-carbonyldiimidazole,stir at room temperature until no bubbles emerge,add 11.6g (113.4mmol) N,O-dimethylhydroxylamine hydrochloride,stir at room temperature for 17 hours.after the reaction mixture was diluted with 150 mL of water,extract with dichloromethane (60mL×3),Dry the organic phase with anhydrous sodium sulfate,filter,remove the solvent under reduced pressure,column chromatography separation,V (petroleum ether): V (ethyl acetate) = 4:1,22.3 g of colorless oily liquid was obtained, and the yield was 94%.

References:

CN111689957,2020,A Location in patent:Paragraph 0038-0042

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