Ethyl chloroformate → Ethyl 4-(cyanomethyl)piperidine-1-carboxylate

HRID 327031

반응식

HRID 327031 반응식
C1(C[N:8]2[CH2:13][CH2:12][CH:11]([CH2:14][C:15]#[N:16])[CH2:10][CH2:9]2)C=CC=CC=1.Cl[C:18]([O:20][CH2:21][CH3:22])=[O:19]>O1CCCC1>[C:15]([CH2:14][CH:11]1[CH2:12][CH2:13][N:8]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:9][CH2:10]1)#[N:16]

참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 5624991-Benzylpiperidine-4-acetonitrile

생성물 1

HCID 18941011Ethyl 4-(cyanomethyl)piperidine-1-carboxylate수율 81.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 25 parts of 1-(phenylmethyl)-4-piperidineacetonitrile in 178 parts of tetrahydrofuran were added dropwise 37.97 parts of ethyl chloroformate at room temperature. The reaction mixture was stirred for 15 hours at room temperature and was then evaporated. The residue was taken up in 90 parts of ethyl acetate and the whole was washed successively with HCl 3N, NaHCO3 and NaCl (sat.). The solvent was evaporated and the residue was distilled (100°-110° C./6.7 Pa), yielding 18.7 parts (81.4%) of ethyl 4-(cyanomethyl)-1-piperidinecarboxylate (interm. 24).

후처리

  1. customwas then evaporated
  2. washthe whole was washed successively with HCl 3N, NaHCO3 and NaCl (sat.)
  3. customThe solvent was evaporated
  4. distillationthe residue was distilled (100°-110° C./6.7 Pa)

출처 및 근거

ORD 기록
ord-6231955ae036458fa3203c65f9c0214e
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05272150

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