HRID27580

反应详情

EQUATION

反应方程式

HRID 27580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

9-(2-Hydroxy-1-propyl)adenine (I, 4.0 g, 20.7 mmol) was suspened in 50% acetic acid (20 ml) and sodium nitrite (4 g, 58 mmol), was slowly added. The mixture was stirred at 25° for 3 hr. The resulting solution was evaporated to dryness and isopropanol added; this operation was repeated once. The solid residue was boiled in isopropanol and filtered. The filtrate was evaporated and crystallized by addition of acetone. Recrystallization was made from iso-propanol/methanol (98:2); a colorless crystalline product was obtained. Yield 3.3 g (82%); M.P. 244°-250°; uv (H2O; pH 5.5), λmax 250 nm.

WORKUP

后处理

  1. customThe resulting solution was evaporated to dryness and isopropanol
  2. additionadded
  3. filtrationfiltered
  4. customThe filtrate was evaporated
  5. customcrystallized by addition of acetone
  6. customRecrystallization
  7. customa colorless crystalline product was obtained