تفاعل #627141

معادلة التفاعل

1,2,3,4-tetrahydro-1-benzazepin-5-one

O-methyl hydroxylamine hydrochloride

sodium acetate

sodium carbonate

→

desired product

المردود 67.7%

(5Z)—N-Methoxy-1,2,3,4-tetrahydro-5H-2-benzazepin-5-imine

المردود 67.7%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed for 3 hours
2. 2
   تركيزThe resulting mixture was concentrated in vacuo
3. 3
   أخرىto remove ethanol
4. 4
   workup.ADDITIONto the residue was added water (15 mL)
5. 5
   استخلاصThe residue in water was extracted with dichloromethane (15 mL×3)
6. 6
   تجفيفdried over sodium sulfate
7. 7
   تركيزconcentrated in vacuo

الإجراء التجريبي

A mixture of 1,2,3,4-tetrahydro-1-benzazepin-5-one (500 mg, 2.530 mmol), O-methyl hydroxylamine hydrochloride (211 mg, 2.530 mmol), sodium acetate (208 mg, 2.530 mmol) and sodium carbonate (536 mg, 5.060 mmol) in ethanol was refluxed for 3 hours. The resulting mixture was concentrated in vacuo to remove ethanol and to the residue was added water (15 mL). The residue in water was extracted with dichloromethane (15 mL×3). The organic layers were combined, dried over sodium sulfate, and concentrated in vacuo to afford 326 mg of the desired product (yield was 67%).

المصدر