Potassium Carbonate → HCID 136341369, compound

HRID 2171336Notes

Reaction equation

HRID 2171336 reaction equation
CS(O[CH2:6][C@@H:7]([NH:9][C:10]1[CH:15]=[C:14]([Cl:16])[N:13]=[C:12](Cl)[N:11]=1)[CH3:8])(=O)=O.C(=O)([O-])[O-:19].[K+].[K+]>O1CCOCC1.O>[Cl:16][C:14]1[CH:15]=[C:10]2[NH:9][C@@H:7]([CH3:8])[CH2:6][N:11]2[C:12](=[O:19])[N:13]=1

Participants

5

Reactant 2

HCID 11430Potassium CarbonateHCID 86728319HCID 86728319, compound

Product 1

HCID 136341369HCID 136341369, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Conditions

Temperature
100 °C

Procedure

To a solution of (S)-2-((2,6-dichloropyrimidin-4-yl)amino)propyl methanesulfonate (1.86 g, 6.20 mmol) and potassium carbonate (2.57 g, 18.6 mmol) in 1,4-dioxane (100 mL) and water (20 mL). The reaction mixture was stirred at 100° C. for 2 h, then concentrated to remove solvent, diluted with water (20 mL), stirred at room temperature for 10 min and filtered. The filter cake was recrystallized with DCM (30 mL) to give the title product.

Workup

  1. concentrationconcentrated
  2. customto remove solvent
  3. additiondiluted with water (20 mL)
  4. stirringstirred at room temperature for 10 min
  5. filtrationfiltered
  6. customThe filter cake was recrystallized with DCM (30 mL)

Sources & evidence

ORD record
ord-fa961ec1028b40a889a2884ece9df8ad
Source dataset
uspto-grants-2015_06
Patent number
US09051325B2

Reaction notes

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