HRID520589

反应详情

EQUATION

反应方程式

HRID 520589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

1-(Phenylsulfonyl)-6-(trimethylstannanyl)-1H-indazol-4-amine (775 mg), Pd(PPh3)4 (212 mg) and 5-bromo-1-[(4-methylphenyl)sulfonyl]-1H-pyrazolo[3,4-b]pyridine (775 mg) were introduced into a microwave vial and DMF (10 ml) was added. The mixture was heated in the microwave at 120° C. for 4 h. The solvent was removed in vacuo and the crude residue was placed on a high vacuum line overnight. The resulting brown oil was purified by FlashMaster II. The crude material was dissolved in chloroform and added to the top of 2×100 g silica SPE cartridges that were subsequently eluted with 0-100% ethyl acetate:cyclohexane over 60 min. The product-containing fractions were combined and the solvent was removed in vacuo. The residue was dried on a high vacuum line to give the title product, 371 mg as a cream solid.

WORKUP

后处理

  1. additionwas added
  2. customThe solvent was removed in vacuo
  3. customwas placed on a high vacuum line overnight
  4. customThe resulting brown oil was purified by FlashMaster II
  5. dissolutionThe crude material was dissolved in chloroform
  6. additionadded to the top of 2×100 g silica SPE cartridges that
  7. washwere subsequently eluted with 0-100% ethyl acetate
  8. customthe solvent was removed in vacuo
  9. customThe residue was dried on a high vacuum line