Hydrochloric Acid → 1-{1-[2-Hydroxy-3-(2-methoxyphenoxy)-propyl]-4-piperidyl}-3-(4-methoxy-phenyl)-imidazolidin-2-one-hydrochloride

HRID 614368노트

반응식

HRID 614368 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:13][CH2:12][N:11]([CH:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)[C:10]2=[O:20])=[CH:5][CH:4]=1.[CH3:21][O:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[O:29][CH2:30][CH:31]1[O:33][CH2:32]1.[ClH:34]>C(O)(C)C>[ClH:34].[OH:33][CH:31]([CH2:30][O:29][C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=1[O:22][CH3:21])[CH2:32][N:17]1[CH2:18][CH2:19][CH:14]([N:11]2[CH2:12][CH2:13][N:9]([C:6]3[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=3)[C:10]2=[O:20])[CH2:15][CH2:16]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 98357((o-Methoxyphenoxy)methyl)oxiraneHCID 233473361-(4-Methoxyphenyl)3-(4-piperidyl)-2-imidazolidinone

생성물 1

HCID 233473501-{1-[2-Hydroxy-3-(2-methoxyphenoxy)-propyl]-4-piperidyl}-3-(4-methoxy-phenyl)-imidazolidin-2-one-hydrochloride

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 17.9 g of 1-[4-methoxy-phenyl)-3-(4-piperidyl)-2-imidazolidinone and 11.7 g of 1-(2-methoxyphenyloxy)-2,3-epoxypropane in 200 ml of isopropyl alcohol is refluxed for 6 hours. The mixture is thereafter acidified with 5N methanolic hydrochloric acid and concentrated under reduced pressure. The residue is freed from moisture still adhering to it by treatment with toluene. Recrystallisation of the residue from methanol with the addition of activated charcoal yields the 1-{1-[2-hydroxy-3-(2-methoxyphenoxy)-propyl]-4-piperidyl}-3-(4-methoxy-phenyl)-imidazolidin-2-one-hydrochloride as a white crystalline substance with a melting point of 214°-215° C.

후처리

  1. temperatureis refluxed for 6 hours
  2. concentrationconcentrated under reduced pressure
  3. customRecrystallisation of the residue from methanol
  4. additionwith the addition of activated charcoal

출처 및 근거

ORD 기록
ord-b2da3d3a4b7b4524a8e73d1382bc0e3e
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144344

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