تفاعل #161241

معادلة التفاعل

Acetyl chloride

8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine

NaHCO3

→

1-(8-nitro-2,3,4,5-tetrahydro-benzo[b]azepin-1-yl)-ethanone

المردود 81.6%

المذيبات

CH2Cl2

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe mixture was filtered
2. 2
   تركيزthe filtrate was concentrated
3. 3
   workup.DISSOLUTIONThe residue was dissolved in CH2Cl2
4. 4
   غسيلwashed with brine
5. 5
   تجفيفdried over Na2SO4
6. 6
   تركيزconcentrated
7. 7
   أخرىThe residue was purified by column chromatography

الإجراء التجريبي

Acetyl chloride (1 g, 13 mmol) was added dropwise to a mixture of 8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.3 g, 6.8 mmol) and NaHCO3 (1 g, 12 mmol) in CH2Cl2 (50 mL). After stirring for 1 h, the mixture was filtered and the filtrate was concentrated. The residue was dissolved in CH2Cl2, washed with brine, dried over Na2SO4 and concentrated. The residue was purified by column chromatography to give 1-(8-nitro-2,3,4,5-tetrahydro-benzo[b]azepin-1-yl)-ethanone as a yellow solid (1.3 g, 80%).

المصدر