HRID1818670

反应详情

EQUATION

反应方程式

HRID 1818670 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

2′-deoxyuridine (4.00 g, 17.5 mmol) and triphenylmethyl chloride (5.37 g, 19.25 mmol) were stirred in anhydrous pyridine (70 ml) at 50° C. overnight. Additional triphenylmethyl chloride (1.00 g, 3.59 mmol) was added after 18 hours, and the mixture was stirred for a further 4 hours at 50° C. The reaction mixture was then poured into ice-H2O (300 ml) and stirred vigorously. The precipitate was extracted with EtOAc (3×100 ml). The organic solution was then washed with 0.5 M HCl (4×100 ml), dried with MgSO4 and filtered. The filtrate was then washed further with EtOAc, which was then evaporated, and finally with DCM. Solvent was removed using a Buchi rotary evaporator, and finally with the vacuum pump.

WORKUP

后处理

  1. stirringstirred vigorously
  2. extractionThe precipitate was extracted with EtOAc (3×100 ml)
  3. washThe organic solution was then washed with 0.5 M HCl (4×100 ml)
  4. dry with materialdried with MgSO4
  5. filtrationfiltered
  6. washThe filtrate was then washed further with EtOAc, which
  7. customwas then evaporated
  8. customSolvent was removed
  9. customa Buchi rotary evaporator