تفاعل #634671

ord-ee4524bbf2b44e3d98424ae55771a645

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe vial was sealed
  2. 2
    أخرىplaced in a 80° C.
  3. 3
    أخرىfor two hours
  4. 4
    غسيلrinsed (3×50 ml) water
  5. 5
    تجفيفdried over magnesium sulfate
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated on a rotary evaporator
  8. 8
    أخرىPurification on a preparative silica gel thin layer chromatography plate (5/95 MeOH/CH2Cl2)

الإجراء التجريبي

To a microwave vial was added 0.032 gm (0.075 mM) 1-[2-(3-Amino-phenyl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl]-2,2-dimethyl-propan-1-one followed by 0.75 ml of 1M tetrabutylammonium fluoride in THF. The vial was sealed and placed in a 80° C. oil bath for two hours then stirred at room temperature overnight. The mixture was diluted with 10 ml ethyl acetate, rinsed (3×50 ml) water, dried over magnesium sulfate, filtered and concentrated on a rotary evaporator. Purification on a preparative silica gel thin layer chromatography plate (5/95 MeOH/CH2Cl2) gave 0.014 gm (64% yield) of 1-[2-(3-Amino-phenyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl]-2,2-dimethyl-propan-1-one, M+1 295, M.P. 239-241° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07939531B2uspto-grants-2011_05