Formaldehyde → 1-Methylpiperidine-2-carboxylic acid

HRID 467553

반응식

HRID 467553 반응식
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[C:7]([OH:9])=[O:8].[CH2:10]=O>C(O)=O>[CH3:10][N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[C:7]([OH:9])=[O:8]

참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 849Pipecolic Acid

생성물 1

HCID 4159391-Methylpiperidine-2-carboxylic acid

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

Into a 25 ml 3-necked round bottom flask, was placed piperidine-2-carboxylic acid (975 mg, 7.56 mmol), HCHO (2.0 ml) and HCOOH (2.6 ml). The resulting solution was allowed to react, with stirring, for 5 hours while the temperature was maintained at reflux. The reaction progress was monitored by LCMS. The mixture was then concentrated by evaporation under vacuum using a rotary evaporator. The residue was triturated with 30 ml of Et2O to provide 1-methylpiperidine-2-carboxylic acid of as a white solid (0.5 g, 41%).

후처리

  1. customInto a 25 ml 3-necked round bottom flask, was placed
  2. customto react
  3. temperaturewas maintained
  4. temperatureat reflux
  5. concentrationThe mixture was then concentrated by evaporation under vacuum
  6. customa rotary evaporator
  7. customThe residue was triturated with 30 ml of Et2O

출처 및 근거

ORD 기록
ord-9fe4d9224b454ca3abf2f191ce757a97
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623871B2

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