HRID410601

反应详情

EQUATION

反应方程式

HRID 410601 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The product of Step 2 (1.45 g, 4.90 mmol) was taken up in CH2Cl2 (30 mL)/MeOH (15 mL), and magnesium monoperoxyphthalate hexahydrate (4.54 g, 7.34 mmol) was added. The reaction was stirred at room temperature for 2 h. The yellow slurry was diluted with aqueous 10% Na2S2O3 and water and extracted with CH2Cl2 (2×). The combined organic layers were washed with saturated aqueous NaHCO3, dried (MgSO4), filtered and evaporated. Flash chromatography (0-50% ethyl acetate in hexanes) afforded methyl 3-{[(5-bromo-1,3-thiazol-2-yl)methyl]sulfonyl}propanoate (1.53 g, 95%) as a white solid. MS ESI: [M+H]+ m/z 327.9/329.9.

WORKUP

后处理

  1. additionwas added
  2. extractionextracted with CH2Cl2 (2×)
  3. washThe combined organic layers were washed with saturated aqueous NaHCO3
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated