* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Stage #1: With triethylamine; 1,1'-carbonyldiimidazole In N,N-dimethyl-formamide at 25 - 60℃; for 0.5 h; Stage #2: at 60℃; for 21 h;
25° C under conditions to N'N- carbonyldiimidazole (205mg, 1.23mmol) and triethylamine (0.26mL,1.84mmol) in anhydrous DMF (6mL) was added dropwise a solution of 1-Boc-2- piperazine carboxylate(250mg, 1.02mmol) in anhydrous DMF (10mL) solution, 60 ° C The reaction 30min, was added anhydrousmethanol (10mL), 60 ° C 21H reaction, the solvent was removed, a saturated sodium chloride solution (10mL× 3) wash Polyester, ethyl acetate (15mL × 2) was extracted, the combined organic phase was dried overanhydrous Na 2 SO 4, the solvent was removed concentrate was subjected to column chromatographySeparation (eluent: Petroleumether / EtOAc (v / v) = 4/1), to give 194mg colorless oil: 1-tert-butoxycarbonyl-2,4-piperazine Acid methyl ester, Yield: 62percent.
Reference：
[1] Patent: CN105399698, 2016, A, . Location in patent: Paragraph 0619; 0620
2
[ 79-22-1 ]
[ 57260-71-6 ]
[ 219509-79-2 ]
Reference：
[1] Bioorganic and Medicinal Chemistry Letters, 2002, vol. 12, # 21, p. 3229 - 3233
[2] Patent: US6335324, 2002, B1, . Location in patent: Page column 67
[3] Bioorganic and Medicinal Chemistry Letters, 2012, vol. 22, # 8, p. 2807 - 2810
[4] Organic and Biomolecular Chemistry, 2012, vol. 10, # 31, p. 6420 - 6431
3
[ 219509-79-2 ]
[ 873697-75-7 ]
Yield
Reaction Conditions
Operation in experiment
99%
With hydrogenchloride In dichloromethane; ethyl acetate at 20℃; for 1 h;
The compound 1-tert-butoxycarbonyl-2,4-piperazine carboxylate (0.18g, 0.61mmol) in dichloromethane(6mL) was added HCl in ethyl acetate solution (4M, 3mL), stirred at rt for 1h, the solvent was removed to give awhite solid 146mg: 1,3-piperazine compound Two carboxylate hydrochloride, yield: 99percent.
Reference：
[1] Patent: CN105399698, 2016, A, . Location in patent: Paragraph 0618; 0622; 0623
methyl 4-(5-((S)-1-aminoethyl)-2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-1,3-oxazole-4-carbonyl)-3-carbamoylpiperazine-1-carboxylate hydrochloride[ No CAS ]
1-(5-((S)-1-aminoethyl)-2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-1,3-oxazole-4-carbonyl)-4-(methoxycarbonyl)piperazine-2-carboxylic acid hydrochloride[ No CAS ]
1-methyl 3-((pivaloyloxy)methyl) 4-(5-((S)-1-aminoethyl)-2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-1,3-oxazole-4-carbonyl)piperazine-1,3-dicarboxylate hydrochloride[ No CAS ]
With hydrogenchloride; In dichloromethane; ethyl acetate; at 20℃; for 1h;
The compound 1-tert-butoxycarbonyl-2,4-piperazine carboxylate (0.18g, 0.61mmol) in dichloromethane(6mL) was added HCl in ethyl acetate solution (4M, 3mL), stirred at rt for 1h, the solvent was removed to give awhite solid 146mg: 1,3-piperazine compound Two carboxylate hydrochloride, yield: 99%.
methyl 4-(5-((S)-1-((tert-butoxycarbonyl)amino)ethyl)-2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-1,3-oxazole-4-carbonyl)-3-carbamoylpiperazine-1-carboxylate[ No CAS ]
1-(5-((S)-1-((tert-butoxycarbonyl)amino)ethyl)-2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-1,3-oxazole-4-carbonyl)-4-(methoxycarbonyl)piperazine-2-carboxylic acid[ No CAS ]
1-methyl 3-((pivaloyloxy)methyl) 4-(5-((S)-1-((tert-butoxycarbonyl)amino)ethyl)-2-(3-(cyclopropylmethoxy)-4-(difluoromethoxy)phenyl)-1,3-oxazole-4-carbonyl)piperazine-1,3-dicarboxylate[ No CAS ]
4-(tert-butoxycarbonyl)piperazine-1-carboxylic acid[ No CAS ]
[ 219509-79-2 ]
Yield
Reaction Conditions
Operation in experiment
62%
25 C under conditions to N'N- carbonyldiimidazole (205mg, 1.23mmol) and triethylamine (0.26mL,1.84mmol) in anhydrous DMF (6mL) was added dropwise a solution of 1-Boc-2- piperazine carboxylate(250mg, 1.02mmol) in anhydrous DMF (10mL) solution, 60 C The reaction 30min, was added anhydrousmethanol (10mL), 60 C 21H reaction, the solvent was removed, a saturated sodium chloride solution (10mL× 3) wash Polyester, ethyl acetate (15mL × 2) was extracted, the combined organic phase was dried overanhydrous Na 2 SO 4, the solvent was removed concentrate was subjected to column chromatographySeparation (eluent: Petroleumether / EtOAc (v / v) = 4/1), to give 194mg colorless oil: 1-tert-butoxycarbonyl-2,4-piperazine Acid methyl ester, Yield: 62%.
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