Formaldehyde → 1-Methylpiperidine-2-carboxylic acid

HRID 467553ノート

反応式

HRID 467553 の反応式
[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]

参加物

4

反応物 2

HCID 712FormaldehydeHCID 849Pipecolic Acid

生成物 1

HCID 4159391-Methylpiperidine-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-9fe4d9224b454ca3abf2f191ce757a97
出典データセット
uspto-grants-2014_01
特許番号
US08623871B2

反応ノート

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