HRID1026677

反应详情

EQUATION

反应方程式

HRID 1026677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of sodium hydride (0.72 g, 17.0 mmol) in dry tetrahydrofuran (40 ml) was added nitromethane (12.4 mmol) at 0° C. temperature. It was further stirred for 30 minutes and then (S)—N-{3-[4-(4-oxo-piperidin-1-yl)-3-fluorophenyl]-2-oxo-oxazolidin-5-ylmethyl}-acetamide (7.2 mmol) was added. The reaction mixture was stirred at 65° C. for 24 hours. The reaction mixture was poured on to crushed ice. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (2×20 ml). The removal of solvent afforded a crude compound, which was purified by column chromatography over silica gel to afford title compound in 17% yield. M.P. 186-187° C. and MS (M+1)=384 (MH+, 100%) M.F.=C18H23FN4O6.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at 65° C. for 24 hours
  2. additionThe reaction mixture was poured on
  3. customto crushed ice
  4. customThe organic layer was separated
  5. extractionthe aqueous layer was extracted with ethyl acetate (2×20 ml)
  6. customThe removal of solvent
  7. customafforded a crude compound, which
  8. customwas purified by column chromatography over silica gel