HRID1160234

反应详情

EQUATION

反应方程式

HRID 1160234 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-(2-tert-butylphenoxy)pyridin-3-amine (1a) (880 mg, 3.6 mmol), benzyl chloroformate (575 uL, 4.0 mmol) and Hunig's base (935 uL, 5.4 mmol) in dichloromethane (9.0 mL) was stirred at rt for 16 h. Saturated ammonium chloride was added and the separated aqueous layer was extracted with dichloromethane (3×15 mL). The combined organic layers were dried (anh. Magnesium sulfate), filtered and evaporated to yield a residue which was purified by reverse phase preparative HPLC. LC-MS m/z 377.1 [M+H]+.

WORKUP

后处理

  1. extractionthe separated aqueous layer was extracted with dichloromethane (3×15 mL)
  2. dry with materialThe combined organic layers were dried (anh. Magnesium sulfate)
  3. filtrationfiltered
  4. customevaporated
  5. customto yield a residue which
  6. customwas purified by reverse phase preparative HPLC