HRID1683307

反应详情

EQUATION

反应方程式

HRID 1683307 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The dimethoxytrityl group of the derivatized CPG from Example 9 is removed by a treatment with 2% dichloroacetic acid followed by washing with dry acetonitrile. The CPG is washed with acetonitrile-pyridine (4:1) followed by a simultaneous treatment of the CPG with 20-30 equivalents of the 10-O-(dimethoxytrityl) decyl-phosphonic acid as the triethylammonium salt, 20-30 equivalents of adamantane carbonyl chloride in acetonitrile-pyridine. The mixture is agitated by circulating the reagents in the synthesis vessel for 10-15 minutes. The CPG is then briefly washed with acetonitrile-pyridine and then treated with diisopropyl phosphite adamantane carbonyl chloride to cap all unreacted hydroxyl groups. Finally, the CPG is washed with acetonitrile-pyridine and then acetonitrile. An estimate of coupling efficiency is derived from the treatment of the CPG with dichloracetic acid in acetonitrile followed by a measurement of the absorbance of an aliquot at 498 nm. Repeating the above procedure n times will yield an oligomer with n+1 decane units and n H-phosphonate linkages. The oligomer is tethered to a LCAA CPG by a succinate group as described above.

WORKUP

后处理

  1. customThe dimethoxytrityl group of the derivatized CPG from Example 9 is removed by a treatment with 2% dichloroacetic acid
  2. washby washing with dry acetonitrile
  3. washThe CPG is washed with acetonitrile-pyridine (4:1)
  4. customfor 10-15 minutes
  5. washThe CPG is then briefly washed with acetonitrile-pyridine
  6. additiontreated with diisopropyl phosphite adamantane carbonyl chloride
  7. customto cap all unreacted hydroxyl groups
  8. washFinally, the CPG is washed with acetonitrile-pyridine