反応 #2253365

反応方程式

ethyl acetate

1,5-Diacetylpyrrolidin-2-one

1,5-diacetylpyrrolidin-2-one

→

5-(1-acetoxyethyl)pyrrolidin-2-one

収率 46.0%

溶媒

acetic acid

反応条件

後処理

1. 1
   workup.DISTILLATIONThis product mixture is distilled at 0.15 mm Hg
2. 2
   その他to give 5.35 g (50 percent)
3. 3
   workup.DISTILLATIONThe residue upon bulb-to-bulb distillation (140° C. bath temperature, 0.15 mm)

実験手順

1,5-Diacetylpyrrolidin-2-one (10.6 g) is hydrogenated at 875 psi at 100° C. over 0.5 g of platinum dioxide in 50 ml of ethyl acetate. The conversion after about 17 hours is about 40 percent. The mixture is freed of the catalyst and solvent and is then hydrogenated again in 50 ml of acetic acid over 1.0 g of platinum dioxide for about 19 hours. The conversion is now about 50 percent by nuclear magnetic resonance analysis. This product mixture is distilled at 0.15 mm Hg to give 5.35 g (50 percent), of unreacted 1,5-diacetylpyrrolidin-2-one. The residue upon bulb-to-bulb distillation (140° C. bath temperature, 0.15 mm) gives 4.85 g (46 percent yield, 92 percent selectivity) of 5-(1-acetoxyethyl)pyrrolidin-2-one, containing a very small amount of 1,5-diacetylpyrrolidin-2-one.

出典