HRID2269578

反应详情

EQUATION

反应方程式

HRID 2269578 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 249 mg of the product of Step 2 in 5 mL of DMF was added 237 mg of n-Bu4NOAc. The reaction mixture was stirred at r.t. for 15 min. Water (20 mL) was added and the product was extracted with 50 mL of EtOAc. The extract was dried over MgSO4 and concentrated in vacuo. The residue was dissolved in 4 mL of THF and 2 mL of MeOH and treated with 1 ml of 1N LiOH. After 12 h, the reaction mixture was treated with 0.2 ml of HOAc and 10 mL of brine. The product was extracted with 40 mL of EtOAc. The extract was dried over MgSO4 and concentrated in vacuo to provide 120 mg of title compound as a white solid.

WORKUP

后处理

  1. extractionthe product was extracted with 50 mL of EtOAc
  2. dry with materialThe extract was dried over MgSO4
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in 4 mL of THF
  5. addition2 mL of MeOH and treated with 1 ml of 1N LiOH
  6. waitAfter 12 h
  7. additionthe reaction mixture was treated with 0.2 ml of HOAc and 10 mL of brine
  8. extractionThe product was extracted with 40 mL of EtOAc
  9. dry with materialThe extract was dried over MgSO4
  10. concentrationconcentrated in vacuo