HRID1005435

反应详情

EQUATION

反应方程式

HRID 1005435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-(Hydroxymethyl)-uracil hydrate 1 (10.00 gm, 0.070 moles) is co-evaporated three times with 50 ml dry pyridine and dissolved in 200 ml dry pyridine at room temperature. Triethylamine (9.8 ml, 0.070 moles) and 4,4'-dimethoxytrityl chloride (23.7 gm, 0.070 moles) are added and the mixture is stirred for 6 hours under a nitrogen atmosphere. Most of the pyridine is removed under reduced pressure and the residue is partitioned between ethyl acetate and saturated sodium bicarbonate. The organic phase is washed twice with saturated sodium chloride, dried over magnesium sulfate, filtered, and evaporated under reduced pressure. The oily residue is triturated with ethyl acetate and hexane to give 5-(4,4'-dimethoxytrityloxymethyl)-uracil 2 as an off-white solid.

WORKUP

后处理

  1. customMost of the pyridine is removed under reduced pressure
  2. customthe residue is partitioned between ethyl acetate and saturated sodium bicarbonate
  3. washThe organic phase is washed twice with saturated sodium chloride
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customThe oily residue is triturated with ethyl acetate and hexane