Methanol → 1-[2-(3-Carbamoyl-4-hydroxyphenoxy)-ethylamino]-3-[3-(1,5-dimethylpyrrol-2-yl)-phenoxy]-2-propanol

HRID 638065노트

반응식

HRID 638065 반응식
[CH3:1][N:2]1[C:6]([CH3:7])=[CH:5][CH:4]=[C:3]1[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH2:15][CH:16]2[O:18][CH2:17]2)[CH:9]=1.[NH2:19][CH2:20][CH2:21][O:22][C:23]1[CH:31]=[C:27]([C:28]([NH2:30])=[O:29])[C:26]([OH:32])=[CH:25][CH:24]=1.CO>C(O)(C)C>[C:28]([C:27]1[CH:31]=[C:23]([CH:24]=[CH:25][C:26]=1[OH:32])[O:22][CH2:21][CH2:20][NH:19][CH2:17][CH:16]([OH:18])[CH2:15][O:14][C:10]1[CH:11]=[CH:12][CH:13]=[C:8]([C:3]2[N:2]([CH3:1])[C:6]([CH3:7])=[CH:5][CH:4]=2)[CH:9]=1)(=[O:29])[NH2:30]

참가 물질

5

반응물 3

HCID 887MethanolHCID 202551361,5-Dimethyl-2-[3-(2,3-epoxypropoxy)-phenyl]-pyrroleHCID 230496945-(2-Aminoethoxy)-2-hydroxybenzamide

생성물 1

HCID 202551411-[2-(3-Carbamoyl-4-hydroxyphenoxy)-ethylamino]-3-[3-(1,5-dimethylpyrrol-2-yl)-phenoxy]-2-propanol

시약·촉매·용매 1

HCID 3776Isopropanol용매2회

실험 절차

Solutions of 5.0 g of crude 1,5-dimethyl-2-[3-(2,3-epoxypropoxy)-phenyl]-pyrrole in 15 ml of isopropanol and of 3.0 g of 5-(2-aminoethoxy)-salicylamide in 30 ml of isopropanol are combined and boiled under reflux for 2.5 hours. A portion of the precipitated reaction product is dissolved by the addition of 50 ml of methanol. The filtered solution is evaporated to dryness and the residue is recrystallised twice from ethyl acetate, yielding 1-[2-(3-carbamoyl-4-hydroxyphenoxy)-ethylamino]-3-[3-(1,5-dimethylpyrrol-2-yl)-phenoxy]-2-propanol having a melting point of 108°-112°.

후처리

  1. temperatureunder reflux for 2.5 hours
  2. customA portion of the precipitated reaction product
  3. customThe filtered solution is evaporated to dryness
  4. customthe residue is recrystallised twice from ethyl acetate

출처 및 근거

ORD 기록
ord-4c5e2b91807f4d00a1bedfc1d7f8310b
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04559354

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