Basic information Safety Supplier Related

4-(4-Bromopyrazol-1-yl)piperidine-1-carboxylic acid tert-butyl ester

Basic information Safety Supplier Related

4-(4-Bromopyrazol-1-yl)piperidine-1-carboxylic acid tert-butyl ester Basic information

Product Name:
4-(4-Bromopyrazol-1-yl)piperidine-1-carboxylic acid tert-butyl ester
Synonyms:
  • 4-(4-Bromo-pyrazol-1-yl)-piperidine-1-carboxylic acid tert-butyl ester
  • Crizotinib Impurity 4
  • CRIXOTINIB-D
  • 4-Bromo-1-(N-boc-piperidin-4-yl)-1H-pyrazole
  • 1-Boc-4-(4-bromo-1-pyrazolyl)piperidine
  • 1-(4-BOC-Piperidino)-4-bromopyrazole
  • (R)-5-broMo-3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-2-a
  • 1-Boc-4-(4-broMopyrazol-1-yl)piperidine
CAS:
877399-50-3
MF:
C13H20BrN3O2
MW:
330.22
Product Categories:
  • intermediate
  • API intermediates
Mol File:
877399-50-3.mol
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4-(4-Bromopyrazol-1-yl)piperidine-1-carboxylic acid tert-butyl ester Chemical Properties

Melting point:
77.0 to 81.0 °C
Boiling point:
411.5±35.0 °C(Predicted)
Density 
1.43
storage temp. 
Keep in dark place,Sealed in dry,Room Temperature
solubility 
soluble in Methanol
form 
Solid
pka
0.92±0.19(Predicted)
color 
Off-white
CAS DataBase Reference
877399-50-3
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Safety Information

Hazard Codes 
Xn
Risk Statements 
22
HS Code 
2933399990
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4-(4-Bromopyrazol-1-yl)piperidine-1-carboxylic acid tert-butyl ester Usage And Synthesis

Synthesis

2075-45-8

141699-59-4

877399-50-3

General procedure for the synthesis of tert-butyl 4-(4-bromopyrazol-1-yl)piperidine-1-carboxylate from 4-bromopyrazole and tert-butyl 4-((methylsulfonyl)oxy)piperidine-1-carboxylate: 2.08 kg of cesium carbonate and 0.78 kg of 4-bromopyrazole were dissolved in 4 liters of N-methyl pyrrolidinone, and heated to 80°C. Subsequently, 2.08 kg of cesium carbonate and 0.78 kg of 4-bromopyrazole were dissolved in 5 liters of N-methyl pyrrolidinone. 1.8 kg of tert-butyl 4-((methylsulfonyl)oxy)piperidine-1-carboxylate was added to the reaction mixture and the reaction lasted for 12 hours. After completion of the reaction, it was cooled to room temperature, 50 liters of methyl tert-butyl ether and 50 liters of water were added and stirred for 1 hour. After separating the organic phase, the organic phase was washed 4 times with 20 liters of water, then dried with 50% hexane and stirred for 2 hours at room temperature. Finally, it was filtered and dried to give 1.35 kg of tert-butyl 4-(4-bromopyrazol-1-yl)piperidine-1-carboxylate in 77% yield.

References

[1] Patent: CN106317024, 2017, A. Location in patent: Paragraph 0060; 0061
[2] Journal of Medicinal Chemistry, 2011, vol. 54, # 12, p. 4092 - 4108
[3] Patent: WO2015/81257, 2015, A2. Location in patent: Page/Page column 81
[4] Tetrahedron Letters, 2014, vol. 55, # 9, p. 1528 - 1531
[5] Patent: US2006/46991, 2006, A1. Location in patent: Page/Page column 64-65

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