Phosphorus oxychloride → 184913-07-3

반응식

[CH3:1][C:2]1[NH:7][C:6](=O)[C:5]2[CH:9]=[CH:10][S:11][C:4]=2[CH:3]=1.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:6]1[C:5]2[CH:9]=[CH:10][S:11][C:4]=2[CH:3]=[C:2]([CH3:1])[N:7]=1

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 18691205HCID 18691205, 화합물

생성물 1

HCID 18691213184913-07-3

실험 절차

A solution of 6.2 g of 6-methylthieno[3,2-c]pyridin-4(5H)-one in 30 ml of phosphoryl chloride was heated under reflux for 1 hour. After being cooled, the excess phosphoryl chloride was removed under reduced pressure, and the residue was poured into ice water, made basic with aqueous 2N sodium hydroxide and extracted with chloroform. The extract was washed successively with water and saturated saline, and dried over anhydrous magnesium sulfate. The drying agent was removed by filtration, and the solvent was removed under reduced pressure to give 7.0 g of 4-chloro-6-methylthieno[3,2-c]pyridine as a brown oily material.

후처리

temperatureunder reflux for 1 hour
temperatureAfter being cooled
customthe excess phosphoryl chloride was removed under reduced pressure
additionthe residue was poured into ice water
extractionextracted with chloroform
washThe extract was washed successively with water and saturated saline
dry with materialdried over anhydrous magnesium sulfate
customThe drying agent was removed by filtration
customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록: ord-c3fc52c9b5b54040add3f3650f04e385
출처 데이터셋: uspto-grants-2000_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06103736

반응 노트

불러오는 중…