Diisopropylethylamine → 3-[5-(2-Acetoxy-2-methyl-propionylamino)-4-carbamoyl-thiophen-2-ylsulfanyl]-propionic acid 2-ethyl-hexyl ester

참여 물질

역할	이름	HCID	투입량
반응물	Diisopropylethylamine	HCID 81531	—
반응물	2-Ethylhexyl 3-mercaptopropionate	HCID 92640	—
반응물	1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)	HCID 636044	—
반응물	[2-[(5-Bromo-3-carbamoyl-2-thienyl)amino]-1,1-dimethyl-2-oxo-ethyl]acetate	HCID 117717729	—
촉매	Bis(dibenzylideneacetone)palladium	HCID 9811564	—
용매	Toluene	HCID 1140	—
생성물	3-[5-(2-Acetoxy-2-methyl-propionylamino)-4-carbamoyl-thiophen-2-ylsulfanyl]-propionic acid 2-ethyl-hexyl ester	HCID 117717785	—

반응 조건

온도	110 °C

반응 단계

Intermediate 11 (1.4 g, 4 mmol) is dissolved in toluene (16 mL) and DIEA (1.4 mL, 8 mmol). Next, Pd2dba3 (110 mg, 0.12 mmol), Xantphos (139 mg, 0.24 mmol) and 3-Mercaptopropionic acid 2-ethylhexylester (1.14 mL, 5 mmol) are added, and the resulting solution is flushed with N2. Reaction mixture is stirred at 110° C. overnight. After evaporation, the crude is purified using column chromatography. The resulting product is obtained as an oil, which crystallised overnight. Obtained product is used as such.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US09382254B2
출처 데이터셋	uspto-grants-2016_07
ORD ID	ord-c686567f3d01469b809b2228195b9e7b
출처 메모	uspto-grants-2016_07