تفاعل #1125653

معادلة التفاعل

7-bromo-8-hydroxymethyl-3,3-dimethyl-3,4-dihydro-1H-quinoxalin-2-one

methyl iodide

carbonate

Ethyl acetate

→

compound

المردود 69.1%

7-Bromo-8-hydroxymethyl-1,3,3-trimethyl-3,4-dihydro-1H-quinoxalin-2-one

المردود 69.1%

المذيبات

water

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىpartitioned
2. 2
   غسيلThe organic layer was washed with saturated brine (10 mL)
3. 3
   تجفيفdried over anhydrous magnesium sulfate
4. 4
   أخرىthe solvent was removed under reduced pressure
5. 5
   أخرىThe obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate)

الإجراء التجريبي

A mixture of 7-bromo-8-hydroxymethyl-3,3-dimethyl-3,4-dihydro-1H-quinoxalin-2-one (Reference Compound No. 5, 62.7 mg, 0.220 mmol), methyl iodide (68.6% L, 1.10 mmol), and cessium carbonate (180 mg, 0.552 mmol) was suspended in anhydrous N,N-dimethylformamide (1 mL) and stirred at room temperature for 2.5 hours. Ethyl acetate (10 mL) and water (10 mL) were added to the reaction mixture and partitioned. The organic layer was washed with saturated brine (10 mL), dried over anhydrous magnesium sulfate, and then the solvent was removed under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate) to give the titled reference compound (45.5 mg) as an orange amorphous product. (Yield 69%)

المصدر