Hydrochloric Acid → (R)-2-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl}-1-methylpyrrolidine hydrochloride

HRID 743323노트

반응식

HRID 743323 반응식
[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][C:12]2[CH:25]=[CH:24][CH:23]=[CH:22][C:13]=2[O:14][CH2:15][C@H:16]2[CH2:20][CH2:19][CH2:18][N:17]2[CH3:21])[CH:7]=[CH:8][CH:9]=1.C(O)C>O1CCOCC1>[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][C:12]2[CH:25]=[CH:24][CH:23]=[CH:22][C:13]=2[O:14][CH2:15][C@H:16]2[CH2:20][CH2:19][CH2:18][N:17]2[CH3:21])[CH:7]=[CH:8][CH:9]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 53979546(R)-2-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl}-1-methylpyrrolidine

생성물 1

HCID 57497641(R)-2-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl}-1-methylpyrrolidine hydrochloride수율 82%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

0.7 ml of a 4N solution of hydrogen chloride in dioxane was added to a solution of 750 mg of (R)-2-{2-[2-(3-methoxyphenyl)ethyl]phenoxymethyl}-1-methylpyrrolidine [prepared as described in step (a) above] in a suitable amount of dioxane, and the resulting mixture was concentrated by evaporation under reduced pressure. The resulting oily residue was dissolved in 10 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 686 mg (yield 82%) of the title compound as a colorless powder, melting at 124°-125° C. [α]D25 -4.2° (c=3.45 ethanol).

후처리

  1. concentrationthe resulting mixture was concentrated by evaporation under reduced pressure
  2. dissolutionThe resulting oily residue was dissolved in 10 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-d5067d392113445b8090c715e442eade
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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