反応 #5030

反応方程式

7-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid

potassium carbonate

methyl iodide

→

compound

収率 100.4%

7-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid methyl ester

収率 100.4%

溶媒

DMF

反応条件

後処理

1. 1
   ろ過After the insoluble matter was filtered off
2. 2
   濃縮the filtrate was concentrated
3. 3
   workup.ADDITIONethyl acetate (500 ml) was added to the residue, which
4. 4
   洗浄was then washed with water
5. 5
   乾燥dried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off

実験手順

7-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine-9-carboxylic acid (6.25 g) was dissolved into DMF (50 ml), to which then potassium carbonate (11 g) and methyl iodide (4.9 ml) were added, and was stirred for 2 hours at room temperature. After the insoluble matter was filtered off and the filtrate was concentrated, ethyl acetate (500 ml) was added to the residue, which was then washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off to give the intended compound 6.65 g (quantitatively) as yellow crystal.

出典