تفاعل #52104

معادلة التفاعل

Diamide

1,7-diacetamido-3,5-dimethyladamantane

diethyene glycol

→

diamine

المردود 70.4%

1,7-diamino-3,5-dimethyladamantane

المردود 70.4%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   استخلاصThe reaction mixture was extracted with a solvent
2. 2
   غسيلThe combined organic solvent was washed with water and brine
3. 3
   تجفيفdried over sodium sulfate
4. 4
   تركيزThe solution was concentrated to approximately 20 mL
5. 5
   workup.ADDITIONAnhydrous hydrogen chloride in ethyl acetate was added
6. 6
   ترشيحThe precipitate was filtered
7. 7
   workup.DISSOLUTIONThe product was then dissolved in water (10 mL)
8. 8
   استخلاصThe product was extracted with ethyl acetate (10 mL×6)
9. 9
   أخرىSolvent was removed

الإجراء التجريبي

Diamide 3 (1.56 g) was added to diethyene glycol (25 mL). The reaction mixture was stirred at 175˜180° C. for 16 h. The brown solution was cooled to room temperature, and water was added (100 mL). The reaction mixture was extracted with a solvent consisting of ethyl acetate (80%) and t-butylmethyl ether (20%) (70 mL×7). The combined organic solvent was washed with water and brine, and dried over sodium sulfate. The solution was concentrated to approximately 20 mL. Anhydrous hydrogen chloride in ethyl acetate was added. The precipitate was filtered. The product was then dissolved in water (10 mL). The product was extracted with ethyl acetate (10 mL×6). Solvent was removed to afford diamine 4 as an off-white solid (767 mg).

المصدر