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ChemicalBook CAS DataBase List 2,6-dichloro-9-(1-methylethyl)-9H-purine
203436-45-7

2,6-dichloro-9-(1-methylethyl)-9H-purine synthesis

8synthesis methods
-

Yield: 77%

Reaction Conditions:

with di-isopropyl azodicarboxylate;triphenylphosphine in tetrahydrofuran at 20; for 24.5 h;

Steps:

1 Synthesis of 2,6-dichloro-9-isopropyl-9H-purine
Synthesis of 2,6-dichloro-9-isopropyl-9H-purine2,6-dichloropurine (2 mmol),Isopropanol (8 mmol)And triphenylphosphine (4 mmol)Was taken up in 40 mL of anhydrous tetrahydrofuran,Then,Diisopropyl azidodicarboxylate (4 mmol)Was added dropwise over 30 minutes at room temperature.Then,The reaction mixture was stirred for a further 24 hours at room temperature.The reaction was monitored periodically by TLC or LC-MS.The reaction mixture was poured into a beaker containing ice cold water.The aqueous layer was extracted three times with 100 mL portions of ethyl acetate,A crude product was obtained.Chromatography on a silica gel column (10 to 80% ethyl acetate in petroleum ether,Gradient elution) to afford2,6-Dichloro-9-isopropyl-9H-purine was obtained with a yield of 77%

References:

Verastem,Inc.;Chen, Ditson;Williams, Meredith JP5746777, 2015, B2 Location in patent:Paragraph 0077