반응 #73030

반응 방정식

4-aminomethyltetrahydropyran-4-ol

4-chloro-3-nitro[1,5]naphthyridine

triethylamine

→

4-[(3-nitro[1,5]naphthyridin-4-ylamino)methyl]tetrahydropyran-4-ol

수율 93.7%

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   농축it was concentrated under reduced pressure
2. 2
   workup.STIRRINGThe residue was stirred with water (300 mL)
3. 3
   기타The resulting solid was isolated by filtration
4. 4
   세척rinsed with water
5. 5
   기타dried in a vacuum oven at 50° C. for 4 hours

실험 절차

A solution of 4-chloro-3-nitro[1,5]naphthyridine (16.6 g, 79.0 mmol) in dichloromethane (250 mL) and triethylamine (14.3 mL, 102.7 mmol) was cooled to 4° C. A solution of 4-aminomethyltetrahydropyran-4-ol (11.4 g, 86.9 mmol) in dichloromethane (70 mL) was added dropwise over a period of 30 minutes. The reaction mixture was allowed to stir at ambient temperature over the weekend and then it was concentrated under reduced pressure. The residue was stirred with water (300 mL). The resulting solid was isolated by filtration, rinsed with water, and dried in a vacuum oven at 50° C. for 4 hours to provide 22.53 g of 4-[(3-nitro[1,5]naphthyridin-4-ylamino)methyl]tetrahydropyran-4-ol.

출처