HRID2180082

反应详情

EQUATION

反应方程式

HRID 2180082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

6-Methyl-5,7,13-triazatetracyclo[9.3.1.02,10.04,8]pentadeca-2(10),3,5,8-tetraene-13-carboxylic acid tert-butyl ester (80 mg, 0.267 mmol) was stirred in 50% aqueous NaOH solution (3 mL) and DMSO (1 mL) then treated with 1-iodopropane (0.03 mL, 0.321 mmol). This mixture was warmed to 40° C. for 2 hours then cooled, treated with H2O and extracted with EtOAc. The organic layer was washed with H2O (3×) then dried (Na2SO4), filtered and concentrated to an oil (90 mg, 0.253 mmol). (TLC 5% MeOH/CH2Cl2 (NH3) Rf 0.15).

WORKUP

后处理

  1. temperaturethen cooled
  2. extractionextracted with EtOAc
  3. washThe organic layer was washed with H2O (3×)
  4. dry with materialthen dried (Na2SO4)
  5. filtrationfiltered