反応 #4889

反応方程式

(S)-malic acid

methylamine

→

(S)-3-Hydroxy-1-methyl-2,5-pyrrolidinedione

溶媒

toluene

反応条件

後処理

1. 1
   その他slowly rose to 50° C
2. 2
   温度After 0.5 hr the stirred mixture was heated
3. 3
   温度to reflux
4. 4
   その他the water was collected in a Dean-Stark trap for 48 hours
5. 5
   その他A total of 93 ml of water was collected
6. 6
   workup.ADDITIONThe toluene residue was treated with 300 ml of ethanol
7. 7
   濃縮concentrated on the rotary evaportor
8. 8
   workup.DISTILLATIONThe residue was distilled
9. 9
   その他The yield of product obtained
10. 10
    その他145°/0.5 mm

実験手順

To a stirred solution of 134 g (1 mole) of (S)-malic acid in 700 ml of toluene was added 97 ml of 40% aqueous methylamine. The temperature slowly rose to 50° C. After 0.5 hr the stirred mixture was heated to reflux and the water was collected in a Dean-Stark trap for 48 hours. A total of 93 ml of water was collected. The toluene residue was treated with 300 ml of ethanol and concentrated on the rotary evaportor. The residue was distilled. The yield of product obtained was 101 g (78%), b.p. 140°/2 mm; 145°/0.5 mm.

出典