Hydrochloric Acid → 3-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}-1-methylpiperidine hydrochloride

HRID 743330노트

반응식

HRID 743330 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH:17]2[CH2:22][CH2:21][CH2:20][N:19]([CH3:23])[CH2:18]2)[CH:6]=[CH:7][CH:8]=1.[ClH:28].C(OCC)(=O)C>O1CCOCC1.CO>[ClH:28].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH:17]2[CH2:22][CH2:21][CH2:20][N:19]([CH3:23])[CH2:18]2)[CH:6]=[CH:7][CH:8]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 100012501-Methyl-3-(2-(4-(3-methoxyphenyl)butyl)phenoxymethyl)piperidine

생성물 1

HCID 100012493-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}-1-methylpiperidine hydrochloride수율 83%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매2회

실험 절차

2.10 g of 3-{2-[4-(3-methoxyphenyl)butyl]phenoxymethyl}-1-methylpiperidine [prepared as described in step (a) above] were dissolved in 10 ml of dioxane, and 1.7 ml of a 4N solution of hydrogen chloride in dioxane was added to the solution, which was shaken and then concentrated by distillation under reduced pressure to give a solid. The solid was dissolved in a small amount of methanol, and then 50 ml of ethyl acetate were added to the solution. The resulting mixture was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 1.92 g (yield 83%) of the title compound as colorless needles, melting at 141°-142.5° C.

후처리

  1. concentrationconcentrated by distillation under reduced pressure
  2. customto give a solid
  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-b067ddbaddfa41c0b09e681211c1de31
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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