反応 #1687631

反応方程式

methanol ether

P2O5

77

N-Methoxycarbonylmethyl-nicotinamide

sodium carbonate

→

5-Methoxy-2-(3-pyridyl)-oxazole

溶媒

water

chloroform

chloroform

反応条件

後処理

1. 1
   ろ過The mixture was filtered
2. 2
   温度after cooling
3. 3
   その他The filtrate was evaporated in vacuo
4. 4
   その他leaving a red oil
5. 5
   抽出Extraction with 3×200 ml of dichloromethane
6. 6
   乾燥drying of the combined organic phases over magnesium sulphate, and removal of the solvent in vacuo
7. 7
   その他gave a red oil which
8. 8
   その他giving a colorless oil, 78

実験手順

A solution of 19.0 g (0.100 mol) of 77 in 300 ml of dry chloroform was refluxed under vigorous stirring with 40 g of P2O5 for 24 h. The mixture was filtered after cooling. The filtrate was evaporated in vacuo leaving a red oil. The precipitate was dissolved in water at 0°-5° C. and the aqueous solution made basic with sodium carbonate. Extraction with 3×200 ml of dichloromethane, drying of the combined organic phases over magnesium sulphate, and removal of the solvent in vacuo gave a red oil which was combined with the above mentioned oil obtained from the chloroform phase. The oil was applied to a silica gel column (eluent; methanol/ether=1/19) giving a colorless oil, 78. Yield: 5.9 g (0.034 mol, 34%).

出典