反応 #82215

反応方程式

4-((amino)thiocarbonyl)morpholine

ethyl bromopyruvate

MgSO4

→

desired compound

収率 55.2%

Ethyl 2-(4-Morpholinyl)thiazole-4-carboxylate

収率 55.2%

溶媒

acetone

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux for 2 h
3. 3
   温度to cool
4. 4
   ろ過filtered
5. 5
   濃縮concentrated in vacuo
6. 6
   洗浄washed with aqueous NaHCO3
7. 7
   乾燥dried over Na2SO4
8. 8
   濃縮concentrated

実験手順

A mixture of 1.85 g (12.7 mmol) of 4-((amino)thiocarbonyl)morpholine, 1.59 ml (12.7 mmol) of ethyl bromopyruvate, and excess MgSO4 in 50 ml of acetone was heated at reflux for 2 h. The resulting mixture was allowed to cool, filtered, and concentrated in vacuo. The residue was taken up in chloroform, washed with aqueous NaHCO3, dried over Na2SO4, and concentrated. Silica gel chromatography using 1% methanol in chloroform provided 1.7 g (55%) of the desired compound, Rf 0.70 (ethyl acetate). Mass spectrum: (M+H)+ =243.

出典