Piperidine → HCID 13557174、化合物

HRID 980207ノート

反応式

HRID 980207 の反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:7]([C:9]1[O:13][N:12]=[CH:11][C:10]=1[C:14](Cl)=[O:15])[CH3:8]>C(#N)C.C(Cl)Cl>[CH2:7]([C:9]1[O:13][N:12]=[CH:11][C:10]=1[C:14]([N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)=[O:15])[CH3:8]

参加物

5

反応物 2

HCID 8082PiperidineHCID 194398045-Ethyl-1,2-oxazole-4-carbonyl chloride

生成物 1

HCID 13557174HCID 13557174、化合物

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

0.2 mol (17.0 g) of piperidine is added dropwise to 0.1 mol (16.0 g) of 5-ethyl-4-isoxazolecarboxylic acid chloride dissolved in 200 ml of acetonitrile, at room temperature with stirring. Stirring is continued for 20 minutes and the mixture is then cooled to room temperature and the piperidine hydrochloride precipitated is filtered off with suction. The filtrate is concentrated under reduced pressure. An oily residue is obtained, and is taken up in 200 ml of methylene chloride, and the mixture is washed first with 100 ml of 2N hydrochloric acid and then with water. After drying over sodium sulfate, the mixture is concentrated under reduced pressure and the oily residue is distilled under reduced pressure (bulb tube distillation). N-(5-Ethyl-4-isoxazolylcarbonyl)-piperidine of boiling point (7 mbar) 90°-110° C. is thus obtained.

後処理

  1. stirringStirring
  2. customthe piperidine hydrochloride precipitated
  3. filtrationis filtered off with suction
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. customAn oily residue is obtained
  6. washthe mixture is washed first with 100 ml of 2N hydrochloric acid
  7. dry with materialAfter drying over sodium sulfate
  8. concentrationthe mixture is concentrated under reduced pressure
  9. distillationthe oily residue is distilled under reduced pressure (bulb tube distillation)

出典と根拠

ORDレコード
ord-fecab3df499b4b7ab77ad2c069f2b6d7
出典データセット
uspto-grants-1987_01
特許番号
US04636513

反応ノート

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