5-(2-Bromoethoxy)salicylamide → Cgp-20712

HRID 638045ノート

反応式

HRID 638045 の反応式
[NH2:1][CH2:2][CH:3]([OH:22])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[N:13]([CH3:21])[CH:14]=[C:15]([C:17]([F:20])([F:19])[F:18])[N:16]=2)=[CH:8][CH:7]=1.Br[CH2:24][CH2:25][O:26][C:27]1[CH:35]=[C:31]([C:32]([NH2:34])=[O:33])[C:30]([OH:36])=[CH:29][CH:28]=1>>[C:32]([C:31]1[CH:35]=[C:27]([CH:28]=[CH:29][C:30]=1[OH:36])[O:26][CH2:25][CH2:24][NH:1][CH2:2][CH:3]([OH:22])[CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([C:12]2[N:13]([CH3:21])[CH:14]=[C:15]([C:17]([F:20])([F:18])[F:19])[N:16]=2)=[CH:10][CH:11]=1)(=[O:33])[NH2:34]

参加物

3

反応物 2

HCID 137544205-(2-Bromoethoxy)salicylamideHCID 202551961-amino-3-[4-(1-methyl-4-(trifluoromethyl)-1H-imidazol-2-yl)-phenoxy]-2-propanol

生成物 1

HCID 2685Cgp-20712

実験手順

A mixture of 1.5 g of 1-amino-3-[4-(1-methyl-4-(trifluoromethyl)-1H-imidazol-2-yl)-phenoxy]-2-propanol and 0.82 g of 5-(2-bromoethoxy)-salicylamide is stirred for 1 hour in an oil bath at a temperature of 100°. The melt is then extracted by boiling with 30 ml of isopropanol. The filtered solution is concentrated to 15 ml, cooled and the crystals that are precipitated are filtered off. Recrystallisation from methanol yields 1-[2-(3-carbamoyl-4-hydroxyphenoxy)-ethylamino]-3-[4-(1-methyl-4-(trifluoromethyl)-1H-imidazol-2-yl)-phenoxy]-2-propanol having a melting point of 195°-197°.

後処理

  1. extractionThe melt is then extracted
  2. concentrationThe filtered solution is concentrated to 15 ml
  3. temperaturecooled
  4. customthe crystals that are precipitated
  5. filtrationare filtered off
  6. customRecrystallisation from methanol

出典と根拠

ORDレコード
ord-6b30949cae6f45b78386ba4048b8c0ef
出典データセット
uspto-grants-1985_12
特許番号
US04559354

反応ノート

読み込み中…