반응 #45103

반응 방정식

tert-butyl 4-cyclobutylpiperazine-1-carboxylate

hydrogen chloride

hydrogen chloride

→

1-cyclobutylpiperazine

수율 85.0%

용매

ethyl acetate

methanol

dioxane

dioxane

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGthe solution was stirred at room temperature for a further 2 h
3. 3
   기타The reaction mixture was evaporated to dryness
4. 4
   기타to afford a solid
5. 5
   기타The crude product was purified by ion exchange chromatography
6. 6
   세척The desired product was eluted from the column
7. 7
   기타were evaporated to dryness

실험 절차

A solution of tert-butyl 4-cyclobutylpiperazine-1-carboxylate (1.1553 g, 4.81 mmol) in ethyl acetate (10 mL) and methanol (10.00 mL) was treated with a 4M-solution hydrogen chloride in dioxane (1.669 mL, 48.07 mmol) was stirred at room temperature for 40 h under nitrogen. The reaction was incomplete so f 4M-solution hydrogen chloride in dioxane (10 mL) was added and the solution was stirred at room temperature for a further 2 h. The reaction mixture was evaporated to dryness to afford a solid. The crude product was purified by ion exchange chromatography, using a SCX column. The desired product was eluted from the column using 3.5M NH3/MeOH and pure fractions were evaporated to dryness to afford 1-cyclobutylpiperazine (0.571 g, 85%) as a yellow oil.

출처