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Hydrochloric Acid → 2-(2-{2-[2-(4-Ethylphenyl)ethyl]phenoxy}-ethyl) piperidine hydrochloride

HRID 743308
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HRID 743308 반응식
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH:10]1[CH2:15][CH2:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[CH2:24][CH2:25][C:26]1[CH:31]=[CH:30][C:29]([CH2:32][CH3:33])=[CH:28][CH:27]=1)=O)(C)(C)C>O1CCOCC1>[ClH:1].[CH2:32]([C:29]1[CH:28]=[CH:27][C:26]([CH2:25][CH2:24][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[O:17][CH2:16][CH2:15][CH:10]2[CH2:11][CH2:12][CH2:13][CH2:14][NH:9]2)=[CH:31][CH:30]=1)[CH3:33]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 194238691-t-Butoxycarbonyl-2-(2-{2-[2-(4-ethylphenyl)ethyl]phenoxy}ethyl)piperidine

생성물 1

HCID 194238282-(2-{2-[2-(4-Ethylphenyl)ethyl]phenoxy}-ethyl) piperidine hydrochloride수율 88%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

5 ml of a 4N solution of hydrogen chloride in dioxane were added to a solution of 0.91 g of 1-t-butoxycarbonyl-2-(2-{2-[2-(4-ethylphenyl)ethyl]phenoxy}ethyl)piperidine [prepared as described in step (a) above] in 5 ml of dioxane, and the resulting solution was allowed to stand at room temperature for 1 hour. At the end of this time, the mixture was concentrated by distillation under reduced pressure, and the resulting oily residue was dissolved in a small amount of ethyl acetate. Diethyl ether was added to the solution, which was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 687 mg (yield 88%) of the title compound as colorless crystals, melting at 74°-76° C.

후처리

  1. concentrationAt the end of this time, the mixture was concentrated by distillation under reduced pressure
  2. dissolutionthe resulting oily residue was dissolved in a small amount of ethyl acetate
  3. additionDiethyl ether was added to the solution, which
  4. customto stand at room temperature
  5. customThe crystals which precipitated
  6. filtrationwere collected by filtration
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-75bc5785889d4156a105d41cca3402e1
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05556864

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