반응 #45176

반응 방정식

Lithium aluminum hydride

1-(1,4-diazepan-1-yl)ethanone

HCl

→

1-ethyl-1,4-diazepane

수율 40.0%

용매

THF

반응 조건

후처리

1. 1
   workup.WAITat 60° C. for 1 h
2. 2
   기타The cooled reaction mixture
3. 3
   workup.ADDITIONwas poured onto ice (500 mL)
4. 4
   기타purified by ion exchange chromatography
5. 5
   세척The desired product was eluted from the column
6. 6
   기타evaporated to dryness

실험 절차

Lithium aluminum hydride (38.2 ml, 38.19 mmol) was added to 1-(1,4-diazepan-1-yl)ethanone (1.697 g, 11.93 mmol) in THF (59.7 ml) at 0° C. under nitrogen. The resulting solution was stirred at ambient temperature for 1 h and then at 60° C. for 1 h. The cooled reaction mixture was poured onto ice (500 mL), acidified with HCl (2M aqueous solution) and purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 7M NH3/MeOH and evaporated to dryness to afford 1-ethyl-1,4-diazepane (0.610 g, 40%) as a yellow liquid. This was used directly with no further purification.

출처