HRID1807046

反应详情

EQUATION

反应方程式

HRID 1807046 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Step C To a solution of 2-(3,6-dihydro-2H-pyran-4-yl)-2-methyl-propionic acid ethyl ester (6 g, 30 mmol) in anhydrous tetrahydrofuran (75 mL) at 0° C. was added a tetrahydrofuran solution (1 M) of LiAlH4 (100 mL, 100 mmol) under nitrogen. The reaction mixture was heated at reflux for 3 h, then cooled to room temperature. Water and aqueous NaOH solution (2N) was added. The mixture was filtered to remove the precipitate, and the filtrate was concentrated. Water was added, and the mixture was extracted with ethyl acetate. The organic layer were separated, washed with water, aqueous HCl solution, brine, dried over MgSO4, and concentrated to give 2-(3,6-dihydro-2H-pyran-4-yl)-2-methyl-propan-1-ol as a brown oil (4.63 g, 98%).

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 3 h
  3. filtrationThe mixture was filtered
  4. customto remove the precipitate
  5. concentrationthe filtrate was concentrated
  6. additionWater was added
  7. extractionthe mixture was extracted with ethyl acetate
  8. customThe organic layer were separated
  9. washwashed with water, aqueous HCl solution, brine
  10. dry with materialdried over MgSO4
  11. concentrationconcentrated