反応 #2006431

反応方程式

NaH

2,2′-biimidazole

DMF

methyl toluenesulfonate

→

1,1′-Dimethyl-2,2′-biimidazole

収率 80.0%

反応条件

後処理

1. 1
   その他over 30 min
2. 2
   workup.WAITat room temperature for 3 h
3. 3
   その他The solvent was removed by vacuum distillation
4. 4
   その他The dark residue was triturated with ether
5. 5
   ろ過suction filtered
6. 6
   その他dried under vacuum
7. 7
   その他The product was purified by sublimation

実験手順

To a stirred solution of 2,2′-biimidazole (Fieselmann, B. F., et al. Inorg. Chem. 17, 2078 (1978)) (4.6 g, 34.3 mmoles) in 100 mL dry DMF in a 250 ml round bottom flask cooled in an ice/water bath was added in portions NaH (60% in mineral oil, 2.7 g, 68.6 mmoles). After the solution was stirred at 0° C. for one hour under N2, methyl toluenesulfonate (10.3 mL, 68.6 mmoles) was added in small portions using a syringe over 30 min. The stiffing of the solution in the ice/water bath was continued for 1 h and then at room temperature for 3 h. The solvent was removed by vacuum distillation. The dark residue was triturated with ether and then suction filtered and dried under vacuum. The product was purified by sublimation. Yield: 80%.

出典