반응 #52104

반응 방정식

Diamide

1,7-diacetamido-3,5-dimethyladamantane

diethyene glycol

→

diamine

수율 70.4%

1,7-diamino-3,5-dimethyladamantane

수율 70.4%

용매

water

반응 조건

후처리

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

실험 절차

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).

출처