Hydrochloric Acid → 2-(2-{2-[2-(3-Hydroxyphenyl)ethyl]phenoxy}ethyl)-1-methylpyrrolidine hydrochloride

HRID 743253노트

반응식

HRID 743253 반응식
COC[O:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH2:17][CH:18]2[CH2:22][CH2:21][CH2:20][N:19]2[CH3:23])[CH:8]=[CH:9][CH:10]=1.[ClH:28]>O1CCOCC1>[ClH:28].[OH:4][C:5]1[CH:6]=[C:7]([CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH2:17][CH:18]2[CH2:22][CH2:21][CH2:20][N:19]2[CH3:23])[CH:8]=[CH:9][CH:10]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 194238962-(2-{2-[2-(3-Methoxymethoxyphenyl)ethyl]phenoxy}ethyl]-1-methylpyrrolidin

생성물 1

HCID 574976172-(2-{2-[2-(3-Hydroxyphenyl)ethyl]phenoxy}ethyl)-1-methylpyrrolidine hydrochloride수율 71%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

1.80 g of 2-(2-{2-[2-(3-methoxymethoxyphenyl)ethyl]phenoxy}ethyl]-1-methylpyrrolidine [prepared as described in step (a) above] were dissolved in 20 ml of a 4N solution of hydrogen chloride in dioxane, and the solution was allowed to stand at room temperature for 30 minutes. At the end of this time, the mixture was concentrated by distillation under reduced pressure, and the resulting oily residue was dissolved in 20 ml of methylene chloride. Ethyl acetate was slowly added to the solution until it just began to show signs of turbidity. The mixture was then allowed to stand overnight at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 1.25 g (yield 71%) of the title compound as colorless crystals, melting at 68°-70° 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 20 ml of methylene chloride
  3. additionEthyl acetate was slowly added to the solution until it
  4. waitto stand overnight at room temperature
  5. customThe crystals which precipitated
  6. filtrationwere collected by filtration
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-99b17066060d41aea1aa08400468b32a
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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