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

HRID 638065ノート

反応式

HRID 638065 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-4c5e2b91807f4d00a1bedfc1d7f8310b
出典データセット
uspto-grants-1985_12
特許番号
US04559354

反応ノート

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