HRID2050031

反应详情

EQUATION

反应方程式

HRID 2050031 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.20 g (6.12 mmol) of 9-(2-benzoyloxyethoxymethyl)-2-methylthioadenine and 100 ml of 40% aqueous methylamine was heated on a steam bath with occasional agitation for one hour. The solution was cooled and spin evaporated in vacuo. The resultant oil was leached with five 40 ml portions of hot ether to give a solid; yield, 1.31 g (84%), m.p. 174°-176°. Recrystallization from ethanol gave the analytical sample of 9-(2-hydroxyethoxymethyl)-2-methylthioadenine, m.p. 175°-176°; λmax (ε×10-3) (10% EtOH in solvent) pH 1-270 (16.7), 291 (sh) (11.9), H2O and pH 13-276 (15.2) nm; nmr (DMSO-d6), 2.49 (3H, S), 3.55 (4H, S), 4.65 (1H, br S), 5.55 (2H, S), 7.31 (2H, S), 8.15 (1H, S) δ .

WORKUP

后处理

  1. temperaturewas heated on a steam bath with occasional agitation for one hour
  2. temperatureThe solution was cooled
  3. customspin evaporated in vacuo
  4. customto give a solid
  5. customyield
  6. customRecrystallization from ethanol