HRID1096854

反应详情

EQUATION

反应方程式

HRID 1096854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A sol. of compound E7 (3.55 mmol; 2.84 g) in MeOH (35.5 mL) was treated with para-toluenesulfonic acid (3.91 mmol; 0.74 g), and the mixture was stirred at rt for 30 min. 10% aq. Na2CO3 (20 mL) was added, and the solvents were partially removed under reduced pressure. The resulting suspension was extracted with EtOAc (200 mL), washed with 10% aq. Na2CO3 (100 mL), sat. aq. NaHCO3 (100 mL), and brine (100 mL). The org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure. The product (2.46 g; 99%) was used for the next step without purification. LC-MS: tR=1.07 min; ES+: 685.50.

WORKUP

后处理

  1. customthe solvents were partially removed under reduced pressure
  2. extractionThe resulting suspension was extracted with EtOAc (200 mL)
  3. washwashed with 10% aq. Na2CO3 (100 mL), sat. aq. NaHCO3 (100 mL), and brine (100 mL)
  4. dry with materialextracts were dried over MgSO4
  5. filtrationfiltered
  6. customthe solvents were removed under reduced pressure
  7. customThe product (2.46 g; 99%) was used for the next step without purification