HRID373276

反应详情

EQUATION

反应方程式

HRID 373276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 17-ethyl-1-hydroxy-12-[2'-(4"-hydroxy-3"-allyloxycyclohexyl)-1'-methylvinyl]-23, 25-dimethoxy-13,19,21,27-tetramethyl-11,28-dioxa-4-azatricyclo[22.3.1.04,9 ]octacos-18-ene-2,3,10,16-tetraone (66 mg) in dry methylene chloride (1.4 ml) was added an excess of diisopropylethyl amine (34 μl) and o-nitrobenzenesulfonyl chloride (36 mg) followed by addition of 4-dimethylaminopyridine (24 mg). The mixture was stirred at room temperature for 18 hours at which time it was diluted with ethyl acetate, extracted from saturated sodium bicarbonate solution and washed with brine. The combined organics were dried over magnesium sulfate and the concentrate purified by flash chromatography on silica gel (ethyl acetate:hexane (1:1)+1% methanol to give the title compound (66 mg).

WORKUP

后处理

  1. extractionextracted from saturated sodium bicarbonate solution
  2. washwashed with brine
  3. dry with materialThe combined organics were dried over magnesium sulfate
  4. customthe concentrate purified by flash chromatography on silica gel (ethyl acetate:hexane (1:1)+1% methanol