HRID243623
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 compound 15 (0.040 g, 0.083 mmol) in methylene chloride (1 mL) was cooled to −30° C. while boron tribromide (0.18 ml) 1M in methylene chloride was added dropwise. After stirring at room temperature for 2 hours, the mixture was cooled to 0° C. and quenched with saturated sodium bicarbonate. The reaction mixture was diluted with ethyl acetate and washed sequentially with saturated NaHCO3, and brine. The organic layer was dried over sodium sulfate and concentrated in vacuo to provide a crude residue which was purified by reverse phase HPLC to afford octanedioic acid hydroxyamide [4-(2-nitro-phenyl)-thiazol-2-yl]-amide 17 (0.018 g, 55% yield).
WORKUP
后处理
- additionwas added dropwise
- temperaturethe mixture was cooled to 0° C.
- customquenched with saturated sodium bicarbonate
- additionThe reaction mixture was diluted with ethyl acetate
- washwashed sequentially with saturated NaHCO3, and brine
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated in vacuo
- customto provide a crude residue which
- customwas purified by reverse phase HPLC