反応 #1876805

反応方程式

hydrochloric acid

5-benzylamino-3-bromo-1-(2′-methoxyethyl)-4-nitropyrazole

→

4,5-diamino-1-(2′-methoxyethyl)pyrazole

4,5-diamino-1-(2′-methoxyethyl)pyrazole dihydrochloride

溶媒

ethanol

反応条件

後処理

1. 1
   その他The catalyst is then removed by filtration
2. 2
   洗浄washed with ethanol
3. 3
   その他the filtrate is evaporated under reduced pressure
4. 4
   その他A crude orange-coloured solid (2.8 g) is thus obtained
5. 5
   その他is triturated in EtOAc (20 ml) for 1 hour
6. 6
   ろ過The solid is then filtered off
7. 7
   洗浄washed with cold EtOAc (20 ml)
8. 8
   その他dried under vacuum

実験手順

A mixture of 5-benzylamino-3-bromo-1-(2′-methoxyethyl)-4-nitropyrazole (4 g, 2.8 mmol) in ethanol (500 ml) containing a 10% Pd/C catalyst (Johnson-Mattey Type 487, dry weight 0.5 g) and 36% hydrochloric acid (0.57 g, 5.6 mmol) is hydrogenated in a Parr Autoclave (1 l) at 1 MPa for 1 hour. The catalyst is then removed by filtration and washed with ethanol, and the filtrate is evaporated under reduced pressure. A crude orange-coloured solid (2.8 g) is thus obtained, and is triturated in EtOAc (20 ml) for 1 hour. The solid is then filtered off and washed with cold EtOAc (20 ml) and then dried under vacuum to give the 4,5-diamino-1-(2′-methoxyethyl)pyrazole in the form of a beige-coloured solid (0.7 g, 27%).

出典