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[ CAS No. 322474-21-5 ] {[proInfo.proName]}

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Chemical Structure| 322474-21-5
Chemical Structure| 322474-21-5
Structure of 322474-21-5 * Storage: {[proInfo.prStorage]}
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Product Details of [ 322474-21-5 ]

CAS No. :322474-21-5 MDL No. :MFCD00239356
Formula : C12H22N2O4S Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 290.38 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 322474-21-5 ]

* 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.

  • Upstream synthesis route of [ 322474-21-5 ]
  • Downstream synthetic route of [ 322474-21-5 ]

[ 322474-21-5 ] Synthesis Path-Upstream   1~3

  • 1
  • [ 18780-70-6 ]
  • [ 322474-21-5 ]
  • [ 24697-74-3 ]
  • [ 1260119-24-1 ]
Reference: [1] European Journal of Medicinal Chemistry, 2011, vol. 46, # 9, p. 3996 - 4009
  • 2
  • [ 24424-99-5 ]
  • [ 2986-19-8 ]
  • [ 173998-77-1 ]
  • [ 322474-21-5 ]
YieldReaction ConditionsOperation in experiment
55% With triethylamine; sodium hydroxide In dichloromethane at 0℃; for 4 h; CH2Cl2 (5 ml) and triethylamine (TEA) (250 l, 1.79mmol) were added to a rapidly stirred solution of Smethylisothioureahemisulfate (500 mg, 3.59 mmol) inNaOH 1N (2.5 ml). The mixture was cooled to T=0°C on an ice bath, and a solution of di-tert-butyl dicarbonate (783.5mg, 3.59 mmol) in CH2Cl2 (2 ml) was added dropwise over 3h. Upon completion of the addition, the mixture was stirredan additional hour, diluted with 1 mL of CH2Cl2, and HCl 1Nwas added until pH 4. The organic layer was extracted withacidic water, and the aqueous layer was separated from theorganic phase and neutralized with NaOH 1N; CH2Cl2 (1 ml)was added and the aqueous phase was extracted twice. Theorganic layers were separated, dried over sodium sulfate,filtered and concentrated under reduced pressure. Diethylether was added and the solvent was evaporated under vacuumtwice. The compound purity was verified by HPLCanalysis as described above. The qualitative analysis of theproduct was finally confirmed by ESI-MS. The product wasthen used directly in the next step. (377 mg, 55 percent)1H NMR (200 MHz, DMSO-d6): 1.39 (s, 9H), 2.45 (s,3H).13C NMR (50 MHz, DMSO-d6): 13.8, 27.8, 79.2, 157.3,161.4.ESI-MS m/z =191 [M+H] +
Reference: [1] Medicinal Chemistry, 2018, vol. 14, # 4, p. 1 - 7
  • 3
  • [ 24424-99-5 ]
  • [ 173998-77-1 ]
  • [ 322474-21-5 ]
Reference: [1] Synthesis, 2012, vol. 44, # 21, p. 3387 - 3391,5
[2] Synthesis (Germany), 2012, vol. 44, # 21, p. 3387 - 3391
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