反応 #73030

反応方程式

4-aminomethyltetrahydropyran-4-ol

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

triethylamine

→

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

収率 93.7%

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   濃縮it was concentrated under reduced pressure
2. 2
   workup.STIRRINGThe residue was stirred with water (300 mL)
3. 3
   その他The resulting solid was isolated by filtration
4. 4
   洗浄rinsed with water
5. 5
   その他dried in a vacuum oven at 50° C. for 4 hours

実験手順

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.

出典