Hydrochloric Acid → HCID 12136903, compound

HRID 1760220Notes

Reaction equation

HRID 1760220 reaction equation
Cl.[NH2:2][C:3]1[C:4]([Cl:10])=[N:5][CH:6]=[N:7][C:8]=1Cl.[NH2:11][C:12]1[CH:13]=[CH:14][C:15]([O:18][CH3:19])=[N:16][CH:17]=1.C(O)C>O>[CH3:19][O:18][C:15]1[N:16]=[CH:17][C:12]([NH:11][C:8]2[C:3]([NH2:2])=[C:4]([Cl:10])[N:5]=[CH:6][N:7]=2)=[CH:13][CH:14]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 794345-Amino-4,6-dichloropyrimidineHCID 811216-Methoxy-3-pyridinylamine

Product 1

HCID 12136903HCID 12136903, compoundYield 53.3%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
130 °C

Procedure

40 mL conc. aqueous hydrochloric acid was added dropwise to 40 g of 5-amino-4,6-dichloropyrimidine and 60.5 g of 5-amino-2-methoxypyridine in 800 ml mixture of ethanol and water (1/1) at room temperature. This mixture was stirred at 130° C. for 7 hours and 20 minutes, and 800 mL water was added to the reaction mixture at room temperature. The resulting suspension was filtered to give crude crystals, and then the crude crystals were subjected to re-crystallization from dimethylformamide and water, to give the title compound (32.7 g, 53% y) as greenish brown crystals. (2) 5-(6-Chloro-9H-9-purinyl)-2-pyridyl methyl ether

Workup

  1. filtrationThe resulting suspension was filtered
  2. customto give crude crystals
  3. customthe crude crystals were subjected to re-crystallization from dimethylformamide and water

Sources & evidence

ORD record
ord-7c43fa72356747bc9a44d05135e13c72
Source dataset
uspto-grants-2005_01
Patent number
US06841549B1

Reaction notes

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