反応 #164172

ord-762ebd227668498f986026cf8361e129

反応方程式

CCOC(=O)C(Br)c1ccccc1
Ethyl 2-bromo-2-phenylacetate
CSc1cccc(N)c1
3-(methylthio)aniline
CCN(C(C)C)C(C)C
DIPEA
CCOC(=O)C(Nc1cccc(SC)c1)c1ccccc1
oil
収率 79.0%
CCOC(=O)C(Nc1cccc(SC)c1)c1ccccc1
(3-methylsulfanyl-phenylamino)-phenyl-acetic acid ethyl ester
収率 79.0%

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Acetonitrile is evaporated
  2. 2
    その他the crude residue is purified by flash chromatography (petroleum ether/EtOAc=85/15)

実験手順

Ethyl 2-bromo-2-phenylacetate (0.22 mL, 1.23 mmol), 3-(methylthio)aniline (0.22 mL, 1.85 mmol), and DIPEA (0.32 mL, 1.85 mmol) are dissolved in acetonitrile (3 mL) and heated under microwave irradiation at 100° C. for 1 hour. Acetonitrile is evaporated and the crude residue is purified by flash chromatography (petroleum ether/EtOAc=85/15) to obtain intermediate I98 as a colorless oil (292 mg, 79% yield).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08835682B2uspto-grants-2014_09