Formic Acid → Methyl 1-Methyl-4-piperidinecarboxylate

HRID 1769042

반응식

HRID 1769042 반응식
[CH3:1][O:2][C:3](=[O:10])[CH:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.[CH:11](O)=O>C=O.O>[CH3:11][N:7]1[CH2:8][CH2:9][CH:4]([C:3]([O:2][CH3:1])=[O:10])[CH2:5][CH2:6]1

참가 물질

5

반응물 2

HCID 284Formic AcidHCID 424914Methyl isonipecotate

생성물 1

HCID 3616844Methyl 1-Methyl-4-piperidinecarboxylate

시약·촉매·용매 2

HCID 712Formaldehyde용매HCID 962Water용매

실험 절차

Dissolve isonipecotic acid methyl ester in formaldehyde (19.4 mL of a 37.5% solution in water, 262 mmol) and treat with formic acid (10.2 mL of a 90% solution, 240 mmol). Heat on a steam bath for 2 hours and evaporate the solvent in vacuo. Dissolve the residue in ethyl ether, dry (MgSO4), filter and evaporate the filtrate in vacuo. Purify by distillation under an argon atmosphere to give 1-methyl-4-piperidinecarboxylic acid, methyl ester as a clear colorless oil (bp 195°-205° C., 760 mm).

후처리

  1. temperatureHeat on a steam bath for 2 hours
  2. customevaporate the solvent in vacuo
  3. dissolutionDissolve the residue in ethyl ether
  4. dry with materialdry (MgSO4)
  5. filtrationfilter
  6. customevaporate the filtrate in vacuo
  7. distillationPurify by distillation under an argon atmosphere

출처 및 근거

ORD 기록
ord-a78b26fd7f6649639b4f072b722cc07a
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05380731

연결된 노트

불러오는 중…