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

HRID 405134

反応式

HRID 405134 の反応式
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

参加物

7

反応条件

温度
45 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-9fe7b119e178466f95b980ab066eb113
出典データセット
uspto-grants-2014_06
特許番号
US08748624B2

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