反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of (S)-(−)-N-[[2-oxo-3-[3-fluoro-4-[1-[(acetoxy)acetyl]-3,6-dihydro-2H-pyridin-4-yl]phenyl]-5-oxazolidinyl]methyl]acetamide (EXAMPLE 39, 475 mg) and anhydrous potassium carbonate (303 mg) in methanol (44 mL) is stirred under N2 at ambient temperature for 1.5 hours and then adjusted to pH 7 with aqueous hydrochloric acid (1M) and concentrated under reduced pressure. The residue is chromatographed on silica gel (230-400 mesh, 40 g), eluting with a gradient of methanol/chloroform (5/95-10/90), and those fractions with an Rf=0.21 by TLC (methanol/chloroform, 10/90) are pooled and concentrated under reduced pressure. The resulting foam is then triturated with methylene chloride/diethyl either and the precipitate filtered to give the title compound, Anal. calcd for C19H22N8O5F: C, 58.31;H, 5.67; N, 10.74. Found: C, 58.15; H, 5.64; N, 10.72.
WORKUP
后处理
- concentrationconcentrated under reduced pressure
- customThe residue is chromatographed on silica gel (230-400 mesh, 40 g)
- washeluting with a gradient of methanol/chloroform (5/95-10/90)
- concentrationconcentrated under reduced pressure
- customThe resulting foam is then triturated with methylene chloride/diethyl either
- filtrationthe precipitate filtered