HRID2240057
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
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
A mixture of 1-[3-(2-chloro-ethoxy)-5-fluoro-2-nitro-phenylmethanesulfonyl]-naphthalene (1.0 g, 2.36 mmoles) in ethanol (25 mL) was stirred under nitrogen in a round bottom flask at 60° C. 10% Pd/C was added, and the temperature was increased to 80° C. Hydrazine hydrate (2.0 mL) was added dropwise and the mixture was stirred at reflux for 3 hours. Reaction mixture was filtered off through Celite, and the solution was washed with H2O (3×), dried over Na2SO4, and concentrated under vacuum to afford the title compound as an off white solid (0.91 g, 2.31 mmoles).
WORKUP
后处理
- temperaturethe temperature was increased to 80° C
- stirringthe mixture was stirred
- temperatureat reflux for 3 hours
- customReaction mixture
- filtrationwas filtered off through Celite
- washthe solution was washed with H2O (3×)
- dry with materialdried over Na2SO4
- concentrationconcentrated under vacuum