Hydrochloric Acid → 1-Benzylpiperidine-4-acetonitrile

HRID 126861

반응식

HRID 126861 반응식
[C:1]([CH:3]([CH:9]1[CH2:14][CH2:13][N:12]([CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:11][CH2:10]1)C(OCC)=O)#[N:2].[OH-].[Na+].Cl>>[C:16]1([CH2:15][N:12]2[CH2:13][CH2:14][CH:9]([CH2:3][C:1]#[N:2])[CH2:10][CH2:11]2)[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 14989188Ethyl alpha-cyano-1-(phenylmethyl)-4-piperidineacetate

생성물 1

HCID 5624991-Benzylpiperidine-4-acetonitrile수율 82%

실험 절차

A mixture of 58 parts of ethyl α-cyano-1-(phenylmethyl)-4-piperidineacetate and 125 parts of sodium hydroxide solution 2 N is stirred for 3 hours at room temperature. The mixture is neutralized with concentrated hydrochloric acid while cooling and the solvent is evaporated. The residue is stirred for 4 hours at 150° C. in 180 parts of N,N-dimethylacetamide. The reaction mixture is cooled, filtered and the filtrate is evaporated. The residue is taken up in water and extracted with methylbenzene. The extract is dried, filtered and evaporated. The residue is distilled, yielding 35 parts (82%) of 1-(phenylmethyl)-4-piperidineacetonitrile; bp. 135°-140° C. at 0.2-0.3 mm. pressure.

후처리

  1. temperaturewhile cooling
  2. customthe solvent is evaporated
  3. stirringThe residue is stirred for 4 hours at 150° C. in 180 parts of N,N-dimethylacetamide
  4. temperatureThe reaction mixture is cooled
  5. filtrationfiltered
  6. customthe filtrate is evaporated
  7. extractionextracted with methylbenzene
  8. customThe extract is dried
  9. filtrationfiltered
  10. customevaporated
  11. distillationThe residue is distilled

출처 및 근거

ORD 기록
ord-a6cd05033ae94af7b28d883d7f3f3e52
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254127

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