Hydrochloric Acid → 1-Cyclobutylpiperazine

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.

1. additionwas added
2. stirringthe solution was stirred at room temperature for a further 2 h
3. customThe reaction mixture was evaporated to dryness
4. customto afford a solid
5. customThe crude product was purified by ion exchange chromatography
6. washThe desired product was eluted from the column
7. customwere evaporated to dryness

ORD 기록

ord-50c919d8e3c1402a8e50a89d94f5007d

출처 데이터셋

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07737149B2