反応 #487543

反応方程式

2,4-dichloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazine

methyl 4-amino-2-(3-chloropropoxy)benzoate

→

methyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)-2-(3-chloropropoxy)benzoate

溶媒

THF

DCM

water

反応条件

後処理

1. 1
   その他The organic layer was collected
2. 2
   乾燥dried over sodium sulfate
3. 3
   濃縮concentrated under vacuum
4. 4
   その他The crude product was purified by silica gel chromatography
5. 5
   その他The product fractions were collected
6. 6
   濃縮concentrated under vacuum

実験手順

To a solution of 2,4-dichloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazine (770 mg, 2.79 mmol) in THF (10 mL) was added methyl 4-amino-2-(3-chloropropoxy)benzoate (681 mg, 2.79 mmol) and Hunig'sBase (1.464 mL, 8.38 mmol). The resulting mixture was stirred for 16 h. The reaction was diluted with DCM and water. The organic layer was collected and dried over sodium sulfate, and concentrated under vacuum. The crude product was purified by silica gel chromatography using 20-40% EtOAc/Hexanes. The product fractions were collected and concentrated under vacuum to give methyl 4-(4-chloro-6-(2,2,2-trifluoroethoxy)-1,3,5-triazin-2-ylamino)-2-(3-chloropropoxy)benzoate as a solid.

出典