HRID849394

反应详情

EQUATION

反应方程式

HRID 849394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Benzenesulphonamide (0.024 g, 0.13 mmol) was added to a solution of Example 26 (0.50 g, 0.12 mmol) and triethylamine (0.019 mL, 0.13 mmol) in CH2Cl2 (1 mL). After stirring for 16 hr, the reaction was diluted with CHCl3 (10 mL) and NaHCO3 (3 mL) and stirred for 30 min. The layers were separated and the aqueous layer was reextracted with CHCl3 (2×20 mL). The combined organic layers were dried over MgSO4, filtered and concentrated. The residue was treated with HCl/ether, a yellow solid was formed which was triturated with ether several times and dried under vacuum to afford Example 54 (0.64.2 g, 83%) as a light brown solid.

WORKUP

后处理

  1. stirringstirred for 30 min
  2. customThe layers were separated
  3. dry with materialThe combined organic layers were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. additionThe residue was treated with HCl/ether
  7. customa yellow solid was formed which
  8. customwas triturated with ether several times
  9. customdried under vacuum
  10. customto afford Example 54 (0.64.2 g, 83%) as a light brown solid