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

HRID 638045노트

반응식

HRID 638045 반응식
[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]

참가 물질

3

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-6b30949cae6f45b78386ba4048b8c0ef
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04559354

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