1-BOC-Piperazine synthesis

11synthesis methods

Product Name:1-BOC-Piperazine
CAS Number:57260-71-6
Molecular formula:C9H18N2O2
Molecular Weight:186.25

110-85-0 Synthesis

110-85-0
563 suppliers
$5.00/5G

24424-99-5 Synthesis

24424-99-5
840 suppliers
$13.50/25G

57260-71-6
739 suppliers
$5.00/5g

Yield:57260-71-6 98.6%

Reaction Conditions:

with formic acid;1-Imino-ethanamine hydrochloride in methanol;lithium hydroxide monohydrate at 20; for 2 h;Reagent/catalyst;Solvent;

Steps:

1-4 Preparation of 1-Boc-piperazine:

Add 10.3 g (0.12 mol) of piperazine to a 500 mL three-necked flask.Add 150 mL of methanol and 150 mL of water and stir until the piperazine is completely dissolved.Add 11.0 g (0.21 mol) of formic acid and stir for 0.5 h.0.11 g (0.0012 mol) of acetamidine hydrochloride catalyst and 8.73 g (0.04 mol) of di-tert-butyl dicarbonate were continuously added, and stirred at room temperature for 2 h.Gas chromatography (GC retention time: raw piperazine 4.3 min;Target product 1-Boc-piperazine: 11.6 min;Impurity by-product 1, 4-bis Boc-piperazine: 17.4 min) detection reaction,After the reaction is completed, the reaction solution is concentrated to recover the solvent.The 165~175oC/5mmHg fraction was collected by distillation under reduced pressure.The target product was obtained in an amount of 22.0 g, and the reaction yield was 98.6%.

References:

CN109970648,2019,A Location in patent:Paragraph 0029-0032