反応 #978520

反応方程式

2-(2,2,2-Trifluoroethyl)-4-chloro-5-[4-(methylsulfonyl)phenyl]-3(2H)-pyridazinone

NaN3

→

2-(2,2,2-Trifluoroethyl)-4-azido-5-[4-(methylsulfonyl)phenyl]-3(2H)-pyridazinone

収率 95.0%

溶媒

DMF

ethyl acetate

反応条件

後処理

1. 1
   洗浄washed with water, 4 times
2. 2
   乾燥dried over MgSO4
3. 3
   ろ過After filtration of the drying agent and concentration of the filtrate in vacuo
4. 4
   その他the residue was purified by chromatography on silica gel (Biotage 40S)
5. 5
   洗浄eluted with 2:1 hexanes-ethyl acetate
6. 6
   その他evaporated

実験手順

2-(2,2,2-Trifluoroethyl)-4-chloro-5-[4-(methylsulfonyl)phenyl]-3(2H)-pyridazinone, prepared according to Example 193E, (500 mg, 1.36 mmol) was dissolved in DMF (10 mL) and treated with NaN3 (100 mg, 1.5 mmol). After 2 hours at room temperature, the reaction was diluted with ethyl acetate and washed with water, 4 times, and dried over MgSO4. After filtration of the drying agent and concentration of the filtrate in vacuo, the residue was purified by chromatography on silica gel (Biotage 40S) eluted with 2:1 hexanes-ethyl acetate. The product fractions were combined and evaporated to provide the azido intermediate, 2-(2,2,2-Trifluoroethyl)-4-azido-5-[4-(methylsulfonyl)phenyl]-3(2H)-pyridazinone (yield: 481 mg, 95%).

出典