Реакция #2161261
ord-e56fe79a6b7b4ec4b73f4b164cfe0b89
Уравнение реакции
2,4,6-trichloropyrimidine
diethylamine
triethylamine
→
(2,6-Dichloro-pyrimidin-4-yl)-diethyl-amine
Реагенты
Нет
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1КонцентрированиеThe mixture was then concentrated
- 2workup.ADDITION25 mL of CH2Cl2 and 25 mL of water were added
- 3ДругоеThe organic layer was separated
- 4Экстракцияthe aqueous layer was extracted by additional amount of dichloromethane (2×10 mL)
- 5Сушкаdried over anhydrous Na2SO4
- 6Концентрированиеconcentrated
- 7ДругоеColumn chromatography on silica gel afforded 1.48 g (62%) of L as colorless solid
Методика
To a stirred solution of 2.0 g (10.90 mmols) of 2,4,6-trichloropyrimidine in 25 mL of anhydrous ethanol at 0° C., was added drop wise a solution 0.79 g (10.90 mmols) of diethylamine in 5 mL of ethanol. This was followed by the addition of 2.3 mL (16.35 mmols) of triethylamine and the mixture was stirred for further 30 min. The mixture was then concentrated and 25 mL of CH2Cl2 and 25 mL of water were added. The organic layer was separated and the aqueous layer was extracted by additional amount of dichloromethane (2×10 mL) and the extracts were combined, dried over anhydrous Na2SO4 and concentrated. Column chromatography on silica gel afforded 1.48 g (62%) of L as colorless solid.