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

関与物質

役割	名称	HCID	仕込み量
反応物	4-Amino-4'-chlorodiphenyl	HCID 8675	—
反応物	Diisopropylethylamine	HCID 81531	—
反応物	Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)	HCID 9886157	—
反応物	2-(6-((2-Carboxyethyl)carbamoyl)pyridin-3-yl)-4-chlorobenzoic acid	HCID 71059998	—
溶媒	Dimethylformamide	HCID 6228	—
溶媒	Ethyl Acetate	HCID 8857	—
生成物	Ethyl 3-(5-(5-chloro-2-((4'-chloro-[1,1'-biphenyl]-4-yl)carbamoyl)phenyl)picolinamido)propanoate	HCID 71059949	—

反応条件

温度	45 °C

反応手順

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.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08748624B2
出典データセット	uspto-grants-2014_06
ORD ID	ord-9fe7b119e178466f95b980ab066eb113
出典メモ	uspto-grants-2014_06