Реакция #5030

Уравнение реакции

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

potassium carbonate

methyl iodide

→

compound

Выход 100.4%

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

Выход 100.4%

Растворители

DMF

Условия реакции

Обработка

1. 1
   ФильтрацияAfter the insoluble matter was filtered off
2. 2
   Концентрированиеthe filtrate was concentrated
3. 3
   workup.ADDITIONethyl acetate (500 ml) was added to the residue, which
4. 4
   Промывкаwas then washed with water
5. 5
   Сушкаdried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off

Методика

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.

Источник