HRID1850403

反应详情

EQUATION

反应方程式

HRID 1850403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10% hydrochloric acid (5 mL) was added to a suspension of acetonitrile (15 mL) containing 5-[4-(4-methoxyphenyl)piperazin-1-yl]-2,2,3,4,6,7-hexamethyl-2,3-dihydro-1-benzofuran-3-ol (1.70 g, 4.14 mmol) obtained in Reference Example 105, and the mixture was stirred at room temperature for 6 hours. The reaction solution was concentrated under reduced pressure, and after that, 10% potassium carbonate aqueous solution was added to the residue so that the aqueous layer became alkaline. Then, extraction was performed using ethyl acetate. The organic layer was washed with water and saturated saline, and then dried using anhydrous sodium sulfate. The solvent was removed under reduced pressure, and the obtained residue was crystallized using ethanol to give 1.50 g of the title compound (yield: 92%)

WORKUP

后处理

  1. customobtained in Reference Example 105
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. additionafter that, 10% potassium carbonate aqueous solution was added to the residue so that the aqueous layer
  4. extractionThen, extraction
  5. washThe organic layer was washed with water and saturated saline
  6. customdried
  7. customThe solvent was removed under reduced pressure
  8. customthe obtained residue was crystallized