反応 #1687627

反応方程式

ethyl acetate

diazomethane

68

4-(3-Pyridyl)-1,2,3-triazole

acetic acid

→

2-Methyl-4-(3-pyridyl)-1,2,3,-triazole

溶媒

ether

ethanol

反応条件

後処理

1. 1
   その他the mixture was evaporated in vacuo
2. 2
   workup.ADDITIONWater (75 ml) was added
3. 3
   抽出Extraction with 3×100 ml of ether
4. 4
   乾燥drying of the organic phase over magnesium sulphate, and removal of the solvent in vacuo
5. 5
   その他gave a brown solid which
6. 6
   その他giving a colorless solid, 69

実験手順

A solution of ca. 3.0 g (0.070 mol) diazomethane in ether was added dropwise to a solution of 6.0 g (0.04 mol) of 68 in 150 ml of ethanol at room temperature. The solution was stirred overnight at ambient temperature. Ca. 1 ml of acetic acid was added and the mixture was evaporated in vacuo. Water (75 ml) was added and the solution made basic with ammonia. Extraction with 3×100 ml of ether, drying of the organic phase over magnesium sulphate, and removal of the solvent in vacuo gave a brown solid which as applied to a silica gel column (eluent: ethyl acetate) giving a colorless solid, 69. Yield: 2.8 g (0.018 mol, 43%).

出典