تفاعل #743022

ord-a151421304e94b5baa9d7ef2028fd486

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGThe reaction was stirred at room temperature for 18 hours
  2. 2
    أخرىsolvent was removed in vacuo
  3. 3
    غسيلThe resultant solid was washed with water
  4. 4
    أخرىpurified by semi-preparative HPLC

الإجراء التجريبي

Title compound 11B, 1-(3-amino-phenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamine (37 mg, 1.1 eq, 0.16 mmol) was added to a solution of 3-methoxypropionic acid (15.5 mg, 1.0 eq, 0.15 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (25 mg, 1.0 eq, 0.16 mmol), 1-hydroxybenzotriazole (20 mg, 1.0 eq, 0.15 mmol) in DMF (1 ml) which had been stirred for 10 minutes under an inert atmosphere. The reaction was stirred at room temperature for 18 hours, after which methanol (1 ml) was added, and solvent was removed in vacuo. The resultant solid was washed with water and purified by semi-preparative HPLC to yield the title compound as a white solid (5.8 mg, 0.02 mmol, 12%). LCMS: [M+H]+=313, Rt=1.35 min, 100% purity.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08071607B2uspto-grants-2011_12