HRID583536
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
The [2-(2-benzoyl-phenyldisulfanyl)-phenyl]-phenyl-methanone (0.55 g, 1.2 mmol) was diluted with ethanol (5 mL) and anhydrous pyridine (5 mL). Hydroxylamine hydrochloride (1 g, 14 mmol) was added and the solution was refluxed for 90 minutes. The solution was cooled and poured into cold aqueous HCl (1N). Ethyl acetate was added, the layers were separated, and the organic portion was washed with brine, dried (MgSO4), and filtered. The filtrate was concentrated to dryness and the residue was triturated with 75% hexane/25% ethyl acetate to give the title compound (0.19 g, 32%) as a white solid, mp 191-193° C.;
WORKUP
后处理
- temperaturethe solution was refluxed for 90 minutes
- temperatureThe solution was cooled
- customthe layers were separated
- washthe organic portion was washed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationThe filtrate was concentrated to dryness
- customthe residue was triturated with 75% hexane/25% ethyl acetate