反応 #161689

反応方程式

2,3-dihydro-1H-indole

2-chloroisonicotinic acid

DIPEA

TBTU

→

(2-chloropyridin-4-yl)-(2,3-dihydroindol-1-yl)-methanone

溶媒

ethyl acetate

THF

反応条件

後処理

1. 1
   洗浄washed with 15% potassium carbonate solution (1×), water (1×) and 1M hydrochloric acid (1×)
2. 2
   その他The organic phase was dried on magnesium sulphate
3. 3
   ろ過filtered
4. 4
   その他evaporated down i
5. 5
   その他The residue was triturated with diisopropylether and suction
6. 6
   ろ過filtered
7. 7
   その他The solid was dried at 40° C. in the circulating air dryer

実験手順

400 μL (3.53 mmol) 2,3-dihydro-1H-indole were added to 500 mg (3.17 mmol) 2-chloroisonicotinic acid, 600 μL (3.49 mmol) DIPEA and 1.10 g (3.43 mmol) TBTU in 20 mL THF. The reaction mixture was stirred overnight, diluted with ethyl acetate and washed with 15% potassium carbonate solution (1×), water (1×) and 1M hydrochloric acid (1×). The organic phase was dried on magnesium sulphate, filtered and evaporated down i. vac. The residue was triturated with diisopropylether and suction filtered. The solid was dried at 40° C. in the circulating air dryer.

出典