HRID41143

反应详情

EQUATION

反应方程式

HRID 41143 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 31 (0.059 g, 0.19 mmol) and Pd on C (10 wt %, 0.006 g) in methanol (3 mL) is stirred at rt for 1 h under 1 atmosphere of hydrogen. The reaction mixture was filtered to remove the catalyst. Water (0.5 mL) and 2 N sodium hydroxide (0.27 mL) were added and the reaction mixture was cooled to 0° C. in an ice-water bath. Then 4-chlorophenylsulfonyl chloride (0.082 g, 0.39 mmol) was added and the reaction mixture was stirred at 0° C. for 4 h and then diluted with ethyl acetate. The organic layer was collected, washed with brine, dried over magnesium sulfate, filtered and evaporated. The residue so obtained was purified by silica gel column chromatography, using ethyl acetate-hexanes 1:1 as eluent, to provide the desired compound. Yield: 22%.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customto remove the catalyst
  3. additionWater (0.5 mL) and 2 N sodium hydroxide (0.27 mL) were added
  4. customThe organic layer was collected
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customThe residue so obtained
  10. customwas purified by silica gel column chromatography