反応 #494964

反応方程式

150a

N-Methoxy-N-methyl-3-nitro-1H-pyrazole-5-carboxamide

→

150b

収率 81.0%

3-Amino-N-methoxy-N-methyl-1H-pyrazole-5-carboxamide

収率 81.0%

溶媒

methanol

反応条件

後処理

1. 1
   その他A 250-mL single-neck round-bottomed flask was purged with nitrogen
2. 2
   その他The mixture was evacuated
3. 3
   workup.ADDITIONcharged with hydrogen gas
4. 4
   その他The hydrogen was then evacuated
5. 5
   workup.ADDITIONnitrogen was charged into the flask
6. 6
   その他The catalyst was removed by filtration through a pad of CELITE®
7. 7
   濃縮The filtrate was concentrated under reduced pressure

実験手順

A 250-mL single-neck round-bottomed flask was purged with nitrogen and charged with 150a (16.0 g, 1.0 eq., 80.0 mmol), 10% palladium on carbon (50% wet, 800 mg), and methanol (100 mL). The mixture was evacuated, charged with hydrogen gas, and stirred under hydrogen atmosphere at room temperature overnight. The hydrogen was then evacuated and nitrogen was charged into the flask. The catalyst was removed by filtration through a pad of CELITE®. The filtrate was concentrated under reduced pressure to afford 150b (11.0 g, 81%) as a white solid. MS-ESI: [M+H]+ 171.1

出典