4-Amino-4'-chlorodiphenyl → Ethyl 3-(5-(5-chloro-2-((4'-chloro-[1,1'-biphenyl]-4-yl)carbamoyl)phenyl)picolinamido)propanoate

HRID 405134

반응식

HRID 405134 반응식
CN(C(ON1N=N[C:11]2C=CC=N[C:10]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[C:25]([CH2:28][CH2:29][NH:30][C:31]([C:33]1[N:38]=[CH:37][C:36]([C:39]2[CH:47]=[C:46]([Cl:48])[CH:45]=[CH:44][C:40]=2[C:41]([OH:43])=O)=[CH:35][CH:34]=1)=[O:32])([OH:27])=[O:26].CCN(C(C)C)C(C)C.[Cl:58][C:59]1[CH:64]=[CH:63][C:62]([C:65]2[CH:70]=[CH:69][C:68]([NH2:71])=[CH:67][CH:66]=2)=[CH:61][CH:60]=1>CCOC(C)=O.CN(C=O)C>[Cl:48][C:46]1[CH:45]=[CH:44][C:40]([C:41](=[O:43])[NH:71][C:68]2[CH:69]=[CH:70][C:65]([C:62]3[CH:61]=[CH:60][C:59]([Cl:58])=[CH:64][CH:63]=3)=[CH:66][CH:67]=2)=[C:39]([C:36]2[CH:35]=[CH:34][C:33]([C:31]([NH:30][CH2:29][CH2:28][C:25]([O:27][CH2:10][CH3:11])=[O:26])=[O:32])=[N:38][CH:37]=2)[CH:47]=1

참가 물질

7

반응 조건

온도
45 °C

실험 절차

Solid HATU (101 mg, 0.27 mmol) was added to a DMF solution (2 mL) of 2-(6-((2-carboxyethyl)carbamoyl)pyridin-3-yl)-4-chlorobenzoic acid (100 mg, 0.27 mmol), i-Pr2NEt (0.2 mL, 1.1 mmol), and 4′-chloro-[1,1′-biphenyl]-4-amine (57 mg, 0.28 mmol) and the resulting mixture was warmed to 45° C. After 16 h the resulting mixture was diluted with EtOAc, washed with water and brine, dried (Na2SO4), concentrated and purified via column chromatography to yield the title compound.

후처리

  1. washwashed with water and brine
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated
  4. custompurified via column chromatography

출처 및 근거

ORD 기록
ord-9fe7b119e178466f95b980ab066eb113
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748624B2

연결된 노트

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