Phosphorus oxychloride → HCID 10845511, 화합물

반응식

O=[C:2]1[C:7]2[CH:8]=[C:9]([C:11]#[N:12])[S:10][C:6]=2[CH:5]=[CH:4][NH:3]1.P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:2]1[C:7]2[CH:8]=[C:9]([C:11]#[N:12])[S:10][C:6]=2[CH:5]=[CH:4][N:3]=1

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 12875894HCID 12875894, 화합물

생성물 1

HCID 10845511HCID 10845511, 화합물

실험 절차

A solution of 4-oxo-4,5-dihydrothieno[3,2-c]pyridine-2-nitrile (500 mg, 2.84 mmol) prepared as in F. Eloy and A. Deryckere, Bull. Soc. Chim. Belg. 1970, 79, 301) and phosphoryl chloride (5 mL) was heated at reflux for 1 hour. The formed red solution was poured onto ice and extracted with methylene chloride (2×150 mL). The dichloromethane solution was dried over anhydrous Na2SO4, filtered, and concentrated. The residue was purified by flash chromatography with 1:10 EtOAc/hexanes to provide the title compound.

후처리

temperatureat reflux for 1 hour
additionThe formed red solution was poured onto ice
extractionextracted with methylene chloride (2×150 mL)
dry with materialThe dichloromethane solution was dried over anhydrous Na2SO4
filtrationfiltered
concentrationconcentrated
customThe residue was purified by flash chromatography with 1:10 EtOAc/hexanes

출처 및 근거

ORD 기록: ord-504480ac02a941da8e2d54e202ede2fc
출처 데이터셋: uspto-grants-2001_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06232320B1

반응 노트

불러오는 중…