反応 #2786

反応方程式

1,2-dibromoethane

sodium azide

DMF

MeLi

azide

→

off-white solid

収率 32.0%

1,2-Bis(methyltriazeno)ethane

収率 32.0%

反応条件

後処理

1. 1
   その他is not evaporated down totally
2. 2
   workup.WAITAfter 3 hr the reaction is worked up
3. 3
   その他is obtained
4. 4
   その他Crystallization from ether/petroleum ether

実験手順

A flask is charged with 5.0 g (27 mmole) of 1,2-dibromoethane, 3.8 g (58 mmole) of sodium azide, and 50 ml of DMF. The mixture is heated at 50° C. with stirring under argon overnight. The mixture is worked up as described above, except that the azide solution is not evaporated down totally. When about 30 ml of solution remains the mixture is treated with 45 ml of a 1.3M solution of MeLi (58 mmole) as above. After 3 hr the reaction is worked up as described above, and a yellow solid is obtained. Crystallization from ether/petroleum ether affords 1.23 g (32% yield) of an off-white solid, mp 64°-6° C. Mass spectra (FAB) Calc (M+H) 145.1201, Found 145.1220±0.0015.

出典