反応 #52104

反応方程式

Diamide

1,7-diacetamido-3,5-dimethyladamantane

diethyene glycol

→

diamine

収率 70.4%

1,7-diamino-3,5-dimethyladamantane

収率 70.4%

溶媒

water

反応条件

後処理

1. 1
   抽出The reaction mixture was extracted with a solvent
2. 2
   洗浄The combined organic solvent was washed with water and brine
3. 3
   乾燥dried over sodium sulfate
4. 4
   濃縮The solution was concentrated to approximately 20 mL
5. 5
   workup.ADDITIONAnhydrous hydrogen chloride in ethyl acetate was added
6. 6
   ろ過The precipitate was filtered
7. 7
   workup.DISSOLUTIONThe product was then dissolved in water (10 mL)
8. 8
   抽出The product was extracted with ethyl acetate (10 mL×6)
9. 9
   その他Solvent was removed

実験手順

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).

出典