HRID1594448

反应详情

EQUATION

反应方程式

HRID 1594448 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To 25 g of methyl 3,4-dihydroxybutanoate was added 250 mL of DCM and stirred to dissolve. 19.8 g of pyridine was added and cooled to 0° C. 41.4 g of trityl chloride was dissolved in 50 mL of DMC and was added at 0-5° C. for 15 minutes. The temperature was allowed to rise to room temperature and was stirred at room temperature for 17 hours. Water was added and the layers were separated. The organic layer was washed with brine, dried and concentrated. The residue was triturated with 25 mL of cyclohexane and the product was purified to give 15 g of the pure product. 1H NMR (CDCl3): 4.25 (m, 1H), 3.6 (s, 3H), 3.15 (d, 2H), 2.5 (m, 2H), 7.2-7.4 (m, 15H).

WORKUP

后处理

  1. dissolutionto dissolve
  2. additionwas added at 0-5° C. for 15 minutes
  3. customto rise to room temperature
  4. stirringwas stirred at room temperature for 17 hours
  5. customthe layers were separated
  6. washThe organic layer was washed with brine
  7. customdried
  8. concentrationconcentrated
  9. customThe residue was triturated with 25 mL of cyclohexane
  10. customthe product was purified