Hydrochloric Acid → Ethyl 4-methylpiperidine-3-carboxylate

HRID 931301ノート

反応式

HRID 931301 の反応式
Cl.[CH3:2][CH:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH:4]1[C:9]([OH:11])=[O:10].[CH2:12](O)[CH3:13]>C(O)(=O)C>[CH3:2][CH:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH:4]1[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 136586094-Methylpiperidine-3-carboxylic acid

生成物 1

HCID 13658603Ethyl 4-methylpiperidine-3-carboxylate

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Hydrogen chloride gas was bubbled into a solution of 4-methylpiperidine-3-carboxylic acid (6.0 g, 41.90 mmol) in ethanol (150 mL) and acetic acid (30 mL) at 0° C. under a nitrogen atmosphere. The reaction mixture was heated at reflux for 48 h, then was cooled and was partitioned between water and ethyl acetate. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to afford ethyl 4-methylpiperidine-3-carboxylate (5.0 g). The material was used without further purification.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 48 h
  3. temperaturewas cooled
  4. customwas partitioned between water and ethyl acetate
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-915fa440dfb3481ebc20e592cac4db4c
出典データセット
uspto-grants-2016_03
特許番号
US09296745B2

反応ノート

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