Реакция #42793

Уравнение реакции

4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine

3-methylpiperidine

→

4-(2-butynyloxy)-5-fluoro-6-(3-methylpiperidino) pyrimidine

Выход 94.0%

Растворители

ethanol

Условия реакции

Обработка

1. 1
   workup.ADDITIONwas added
2. 2
   Температураunder reflux condition
3. 3
   Концентрированиеconcentrated
4. 4
   workup.ADDITIONInto the residue was added a saturated ammonium chloride aqueous solution
5. 5
   Экстракцияthe mixture was extracted with tert-butyl methyl ether three times
6. 6
   ПромывкаThe organic layers were washed with a saturated sodium chloride aqueous solution
7. 7
   Сушкаdried over anhydrous magnesium sulfate
8. 8
   Концентрированиеconcentrated

Методика

Into 3 ml of ethanol was resolved 0.3 g of 4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine, 0.45 g of 3-methylpiperidine was added therein, and the mixture was stirred for 10 hours under reflux condition. The reaction mixture was cooled to near room temperature, and concentrated. Into the residue was added a saturated ammonium chloride aqueous solution, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.37 g of 4-(2-butynyloxy)-5-fluoro-6-(3-methylpiperidino) pyrimidine (hereinafter, referred to as Compound (3)).

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