HRID849141

反应详情

EQUATION

反应方程式

HRID 849141 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title material of Example 201 in formic acid is added to a solution of hydroxylamine-O-sulfonic acid in formic acid over a 5 min. period with stirring under N2. The mixture is heated under reflux for 3 hours and then cooled to room temperature. The reaction is quenched with cold water and the solution is neutralized with 6N NaOH. It is then extracted three times with CH2Cl2. The combined organic layers are dried over MgSO4 and the solvent is removed on a rotary evaporator. The desired products are purified and isolated by HPLC to give both the 3- and 7-substituted title products.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 3 hours
  3. customThe reaction is quenched with cold water
  4. extractionIt is then extracted three times with CH2Cl2
  5. dry with materialThe combined organic layers are dried over MgSO4
  6. customthe solvent is removed on a rotary evaporator
  7. customThe desired products are purified
  8. customisolated by HPLC
  9. customto give both the 3- and 7-substituted title products