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Chemical Structure| 1052714-60-9 Chemical Structure| 1052714-60-9

Structure of 1052714-60-9

Chemical Structure| 1052714-60-9

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Product Details of [ 1052714-60-9 ]

CAS No. :1052714-60-9
Formula : C15H22ClN3O4S
M.W : 375.87
SMILES Code : O=C(OC(C)(C)C)N(C(OC(C)(C)C)=O)C1=NC(SC)=NC(Cl)=C1

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Application In Synthesis of [ 1052714-60-9 ]

* 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.

  • Downstream synthetic route of [ 1052714-60-9 ]

[ 1052714-60-9 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 24424-99-5 ]
  • [ 1005-38-5 ]
  • [ 309256-03-9 ]
  • [ 1052714-60-9 ]
YieldReaction ConditionsOperation in experiment
With dmap; potassium carbonate; In tetrahydrofuran; at 25 - 35℃; 6.1[00232] Reagents:[00233]; Experimental procedure; .bul. Charge 4-Amino-6-chloro-2-(methylthio)pyrimidine and THF into a clean and dry round bottom flask at 25-35 °C..bul. Add K2C03 lot wise at 25-35 ° C in 5-10 minutes..bul. Add Boc anhydride slowly at 25-35 °C in 15-30 minutes..bul. Stir at 25-35 °C for 15-30 minutes..bul. Add DMAP slowly in 5-10 minutes at 25-35 °C..bul. Maintain the reaction mass at 25-35 °C for 1-2 hours..bul. Check the progress of reaction by TLC..bul. Upon completion, charge ethyl acetate and water..bul. Stir the reaction mass at 25-35 °C for 10-15 minutes. .bul. Separate the aqueous layer and organic layer..bul. Wash the organic layer with saturated sodium chloride solution..bul. Dry the organic layer over sodium sulphate.bul. Filter sodium sulphate out.bul. Wash the sodium sulphate with Ethyl acetate..bul. Concentrate the organic layer completely under vacuum..bul. Yield: 632 g.bul. percent of Yield: 98.46..bul. Purity by HPLC: 77.98percent Di-Boc compound..bul. 11.49percent Mono Boc compound.Alternatively, compound 6.1 can be prepared by addition of (BOC)2NH anion to the corresponding 4,6-dichloropyrimidine or other suitable methods known in the art.
  • 2
  • [ 24424-99-5 ]
  • [ 1005-38-5 ]
  • [ 1052714-60-9 ]
YieldReaction ConditionsOperation in experiment
66% With dmap; In dichloromethane; at 20℃; for 12.5h; Step 1. A solution of <strong>[1005-38-5]4-amino-6-chloro-2-methylthiopyrimidine</strong> (8.64 g, 49.2mmol) and 4-dimethylaminopyridine (636 mg, 5.21 mmol) in dichloromethane (60 mL) was treated with di-tert-butyl dicarbonate (23.6 g, 108 mmol) in small portions over 30 minutes. The solution was allowed to stir at ambient temperature for 12 hours, was diluted with dichloromethane (150 mL), washed twice with water (200 mL) followed by saturated brine (100 mL), dried over Na2SO4, then filtered and the remaining liquid evaporated. Theresulting solid was triturated with 1:1 pentane:ether, collected by filtration and dried under vacuum to afford 4-bis(tert-butoxycarbonyl)amino-6-chloro-2-methylthiopyrimidine as a waxy off-white solid (12.19 g, 32.4 mmol, 66percent); m.p. 90-9 1 °C; TLC RF 0.30 (10:90 ethyl acetate-hexane). 1H NMR (500 MHz, CDC13) oe 7.48 (1H, s), 2.49 (3H, s), 1.55 (18H, s).
 

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