Реакция #657878

Уравнение реакции

water

3-(methylsulfanyl)propan-1-ol

sodium hydride

2-(propylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

→

title compound

2-[3-(methylsulfanyl)propoxy]-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione

Растворители

tetrahydrofuran

Условия реакции

Обработка

1. 1
   workup.STIRRINGthe mixture was stirred at room temperature for 5 hr
2. 2
   Экстракцияthe mixture was extracted with ethyl acetate
3. 3
   ПромывкаThe extract was washed with saturated brine
4. 4
   Сушкаdried over anhydrous magnesium sulfate
5. 5
   ДругоеThe solvent was evaporated under reduced pressure
6. 6
   ДругоеThe residue was purified by silica gel column chromatography (acetic acid ethyl/hexane)

Методика

To a suspension of sodium hydride (60% in oil, 48 mg) in tetrahydrofuran (5 ml) was added 3-(methylsulfanyl)propan-1-ol (0.206 ml) at room temperature, and the mixture was stirred at room temperature for 10 min. To the reaction mixture was added 2-(propylsulfanyl)-3-[4-(2,2,2-trifluoroethoxy)phenyl]pyrido[2,3-d]pyrimidine-4,7(3H,8H)-dione (165 mg), and the mixture was stirred at room temperature for 5 hr. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (acetic acid ethyl/hexane) to give the title compound (96 mg).

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