Ethyl Bromide → 6-Bromo-8-ethyl-2-methylsulfanylpyrido[2,3-d]pyrimidin-7-one

To a suspension of NaH (60%, 0.15 g, 3.75 mmol) in anhydrous dimethylformamide (10 mL) was added 6-bromo-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one (0.68 g, 2.50 mmol) at room temperature and the reaction was stirred at 50° C. for 0.5 h. The reaction mixture was cooled down to room temperature and ethyl bromide (0.22 mL, 0.32 g, 2.93 mmol) was added and stirred at 50° C. for 1.5 h. After completion, the mixture was poured onto ice water (10 g), and the white precipitate was filtered off to give 6-bromo-8-ethyl-2-(methylthio)pyrido[2,3-d]pyrimidin-7(8H)-one (0.57 g, 1.90 mmol, 76%). ESMS m/z 300 (M+H)+.

1. temperatureThe reaction mixture was cooled down to room temperature
2. stirringstirred at 50° C. for 1.5 h
3. additionAfter completion, the mixture was poured onto ice water (10 g)
4. filtrationthe white precipitate was filtered off

ORD 기록

ord-d6d9e9336d9c4b1299967c28c3e3ee53

출처 데이터셋

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08674095B2