反応 #161730

反応方程式

4,5-difluoroindoline hydrochloride

4-chloropicolinic acid

TBTU

→

(4-chloro-pyridin-2-yl)-(4,5-difluoro-2,3-dihydro-indol-1-yl)-methanone

溶媒

DMF

反応条件

後処理

1. 1
   抽出extracted successively with a 15% potassium carbonate solution, water
2. 2
   その他The organic phase was dried
3. 3
   ろ過filtered
4. 4
   濃縮concentrated to dryness by rotary evaporation
5. 5
   workup.STIRRINGThe residue was stirred with diisopropylether
6. 6
   ろ過filtered
7. 7
   その他dried

実験手順

0.50 g (3.2 mmol) 4-chloropicolinic acid, 1.1 g (3.4 mmol) TBTU and 0.91 mL (6.5 mmol) TEA were placed in 10 mL DMF. 0.63 g (3.3 mmol) 4,5-difluoroindoline hydrochloride were added. The reaction mixture was stirred overnight at RT and then extracted successively with a 15% potassium carbonate solution, water, a 1M HCl solution and EtOAc. The organic phase was dried, filtered and concentrated to dryness by rotary evaporation. The residue was stirred with diisopropylether and the undissolved solid was suction filtered and dried.

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