反応 #674322

反応方程式

triazine

3-[(4-Chloro-1,3,5-triazin-2-yl)amino]benzenemethanesulfonamide

K2CO3

4,4-difluoropiperidine hydrochloride

→

title compound B2

3-[(4-(4,4-Difluoropiperidin-1-yl)-1,3,5-triazin-2-yl)amino]-benzenemethanesulfonamide

溶媒

DMSO

EtOAc

反応条件

後処理

1. 1
   温度After cooling to room temperature it
2. 2
   抽出extracted with water
3. 3
   洗浄The organic layer was washed with brine
4. 4
   乾燥dried over MgSO4
5. 5
   濃縮concentrated under reduced pressure
6. 6
   workup.STIRRINGThe residue was stirred with DCM

実験手順

To a solution of triazine A1 (270 mg, 0.9 mmol) in DMSO (0.9 mL) were added K2CO3 (370 mg, 2.7 mmol) and 4,4-difluoropiperidine hydrochloride (140 mg, 0.9 mmol). The mixture was stirred for 2 hours at 80° C. After cooling to room temperature it was diluted with EtOAc and extracted with water. The organic layer was washed with brine, dried over MgSO4 and concentrated under reduced pressure. The residue was stirred with DCM to give the solid title compound B2 which was isolated by filtration and dried in vacuo (white powder, 110 mg, 32%). 1H NMR (300 MHz, d6-DMSO, 300K) δ 1.90-2.15 (m, 4H), 3.81-3.98 (m, 4H), 4.21 (s, 2H), 6.88 (s, 2H), 6.98-7.04 (m, 1H), 7.21-7.34 (m, 1H), 7.44-7.60 (m, 1H), 7.78-7.90 (m, 1H), 8.25 (s, 1H), 9.77 (s, 1H). MS (ES) C15H18F2N6O2S requires: 384. found: 385 (M+H)+.

出典