反応 #1008

反応方程式

4-Methoxy-3-nitropyridine

methylamine

→

4-methylamino-3-nitropyridine

収率 88.0%

溶媒

EtOH

EtOH

EtOH

反応条件

後処理

1. 1
   その他The bomb was sealed
2. 2
   その他lowered into an oil bath at 120° C
3. 3
   その他fell to 90° C.
4. 4
   その他for 2 hours
5. 5
   その他(not very soluble) and the solvent was evaporated

実験手順

4-Methoxy-3-nitropyridine (8.17 g, 53.0 mmol) was transferred to a bomb in EtOH (5-10 mL). To this was added a solution of methylamine in EtOH (26.4 mL, 8.03M, 0.212 mol). The bomb was sealed and lowered into an oil bath at 120° C. The bath temperature fell to 90° C. and remained that way for 2 hours. The temperature was raised to 140° C. over 0.5 hour and held there 0.5 hour. The contents were transferred to a flask with EtOH (not very soluble) and the solvent was evaporated. Flash chromatography on silica gel with a gradient of CH2Cl2 /CH3OH gave 7.17 g (88%) of 4-methylamino-3-nitropyridine as a yellow solid: mp 155°-158° C.

出典