تفاعل #66588

معادلة التفاعل

Acetic acid trifluoroacetic acid

2-(3,4-dimethoxyphenyl)ethanamine

hexamethylenetetramine

→

title product

المردود 95.0%

6,7-Dimethoxy-3,4-dihydroisoquinoline

المردود 95.0%

المذيبات

water

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المعالجة

1. 1
   درجة الحرارةThe resulting solution was heated
2. 2
   درجة الحرارةat reflux for about 5 hours in an oil bath
3. 3
   استخلاصthe solution was extracted with dichloromethane (3×200 mL)
4. 4
   تجفيفdried over anhydrous sodium sulfate
5. 5
   أخرىSolids were removed by filtration
6. 6
   تركيزthe resulting filtrate was concentrated in vacuo

الإجراء التجريبي

Acetic acid/trifluoroacetic acid (100 mL) was added to a solution of 2-(3,4-dimethoxyphenyl)ethanamine (20 g, 110.38 mmol, 1.00 equiv) and hexamethylenetetramine (31 g, 221.11 mmol, 2.00 equiv). The resulting solution was heated at reflux for about 5 hours in an oil bath. After adding water (100 mL), the solution was extracted with dichloromethane (3×200 mL), and the organic layers were combined and dried over anhydrous sodium sulfate. Solids were removed by filtration, and the resulting filtrate was concentrated in vacuo to give the title product as a yellow oil (20 g, yield=95%). LC-MS: m/z=192 (MH)+.

المصدر