反应 #1687633
ord-f52cc74625a44273a77af5187dab8ebb
反应方程式
methyl nicotinoate
2-amino-2,2,dimethyl-ethanol
water
→
4,4-Dimethyl-2-(3-pyridyl)-oxazoline
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他The solvent was removed in vacuo, 300 ml of water
- 2workup.ADDITIONadded
- 3萃取the aqueous solution extracted with 3×300 ml of dichloromethane
- 4干燥Drying of the organic phase over magnesium sulphate and evaporation in vacuo
- 5其他gave a red oil which
- 6过滤was filtered through silica gel (eluent: methanol/ether=1/19)
- 7其他Removal of solvents in vacuo
- 8其他gave a yellow oil, 86
实验过程
A solution of 69 g (0.500 mol) of methyl nicotinoate and 45 g (0.500 mol) of 2-amino-2,2,dimethyl-ethanol in 600 ml of toluene was refluxed with a water separator overnight. The solvent was removed in vacuo, 300 ml of water added, and the aqueous solution extracted with 3×300 ml of dichloromethane. Drying of the organic phase over magnesium sulphate and evaporation in vacuo gave a red oil which was filtered through silica gel (eluent: methanol/ether=1/19). Removal of solvents in vacuo gave a yellow oil, 86. Yield: 30.0 g (0.170 mol, 34%).