反応 #2358604

反応方程式

3-tert-butyl-1H-pyrazole-5-carbonitrile

phenylsulfonyl chloride

ethyl acetate hexane

→

required product

(3-tert-butyl-1-(phenylsulfonyl)-1H-pyrazol-5-yl)methanamine

溶媒

dichloromethane

反応条件

後処理

1. 1
   workup.ADDITIONwas added to reaction mixture, organic layer
2. 2
   その他was separated
3. 3
   洗浄washed with 1N HCl (2×20 ml
4. 4
   乾燥Dried the contents over sodium sulfate
5. 5
   濃縮concentrated under reduced pressure
6. 6
   その他the crude obtained
7. 7
   その他was recrystallised from hexane

実験手順

To a stirred solution of 3-tert-butyl-1H-pyrazole-5-carbonitrile (3 g, 20 mmol) in dichloromethane (30 ml, 10 times) TEA (2.44 g (3.36 ml), 24 mmol, 1.2 eq) was added at 00° C. Then phenylsulfonyl chloride (2.84 g (2 ml), 10 mmol, 0.8 eq) was added at 00° C. and the reaction mass was stirred for 12 h at room temperature. Progress of the reaction was monitored by TLC (20% ethyl acetate-hexane, Rf˜0.6). On completion of the reaction, ice water (20 ml) was added to reaction mixture, organic layer was separated and washed with 1N HCl (2×20 ml followed by with water (2×15 ml), Dried the contents over sodium sulfate, concentrated under reduced pressure and the crude obtained was recrystallised from hexane to yield the required product as an off white solid (4 g, 68%).

出典