Реакция #332313

Уравнение реакции

4-pyridinepropanol

4-(1-pyrrolidinyl)pyridine

methacrylic acid

N,N′-dicyclohexylcarbodiimide

→

4-pyridinepropanol methacrylate

Растворители

dichloromethane

Условия реакции

Обработка

1. 1
   Другоеto react at room temperature for 1 hour
2. 2
   ДругоеThen, insoluble urea was removed by filtration
3. 3
   Другоеfollowed by removal of solvent under reduced pressure
4. 4
   ДругоеThe residual material was purified by column chromatography (column: silica (manufactured by WAKO Co.), solvent: hexane/ethyl acetate)

Методика

After 6.85 g (50 mmol) of 4-pyridinepropanol (manufactured by Aldrich Co.) represented by formula (19), 4.73 g (55 mmol) of methacrylic acid (manufactured by Aldrich Co.) represented by formula (20), and 740 mg (5 mmol) of 4-(1-pyrrolidinyl)pyridine (manufactured by Aldrich Co.) were dissolved in 100 ml of dehydrated dichloromethane (manufactured by WAKO Co.), 11.3 g (55 mmol) of N,N′-dicyclohexylcarbodiimide (DCC) (manufactured by Aldrich Co.) was added thereto and allowed to react at room temperature for 1 hour. Then, insoluble urea was removed by filtration, followed by removal of solvent under reduced pressure. The residual material was purified by column chromatography (column: silica (manufactured by WAKO Co.), solvent: hexane/ethyl acetate) to obtain 4-pyridinepropanol-methacrylate represented by formula (21) (yield amount: 8.5124 g, yield rate: 82.8%). The reaction scheme is shown below.

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