Hydrochloric Acid → 3-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}piperidine hydrochloride

HRID 743328노트

반응식

HRID 743328 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH2:22][CH2:23][CH2:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([O:32][CH3:33])[CH:27]=2)[CH2:9]1)=O)(C)(C)C.[ClH:34]>O1CCOCC1>[ClH:34].[CH3:33][O:32][C:28]1[CH:27]=[C:26]([CH2:25][CH2:24][CH2:23][CH2:22][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[O:15][CH2:14][CH:10]2[CH2:11][CH2:12][CH2:13][NH:8][CH2:9]2)[CH:31]=[CH:30][CH:29]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 106473391-t-Butoxycarbonyl-3-{2-[4-(3-methoxyphenyl)butyl]phenoxymethyl}piperidine

생성물 1

HCID 574976463-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}piperidine hydrochloride수율 85%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

1.79 g of 1-t-butoxycarbonyl-3-{2-[4-(3-methoxyphenyl)butyl]phenoxymethyl}piperidine [prepared as described in step (a) above] were dissolved in 5 ml of dioxane and 5 ml of a 4N solution of hydrogen chloride in dioxane were added to the solution. The mixture was allowed to stand at room temperature for 2 hours, after which the solvent was removed by distillation under reduced pressure. The resulting residue was dissolved in 20 ml of ethyl acetate, and the solution was allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 1.31 g (yield 85%) of the title compound as needles, melting at 136°-137° C.

후처리

  1. customafter which the solvent was removed by distillation under reduced pressure
  2. dissolutionThe resulting residue was dissolved in 20 ml of ethyl acetate
  3. customto stand at room temperature
  4. customThe crystals which precipitated
  5. filtrationwere collected by filtration
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-70a3b5a7eaa148fbbea063fc24065d75
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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