Formic Acid → Methyl 1-Methyl-4-piperidinecarboxylate

HRID 1769042ノート

反応式

HRID 1769042 の反応式
[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

参加物

5

反応物 2

HCID 284Formic AcidHCID 424914Methyl isonipecotate

生成物 1

HCID 3616844Methyl 1-Methyl-4-piperidinecarboxylate

試薬・触媒・溶媒 2

HCID 712Formaldehyde溶媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-a78b26fd7f6649639b4f072b722cc07a
出典データセット
uspto-grants-1995_01
特許番号
US05380731

反応ノート

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