HRID619897
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
To a solution of 2-aminothiophenol (90%, 100 g, 0.72 mol) and sodium hydroxide (31.7 g, 0.792 mol) in 90% aqueous ethanol (500 ml) was added dropwise 2-bromopropane (89 g, 0.72 mol) at room temperature. When the addition was complete, the reaction mixture was refluxed for 3 hours, cooled to room temperature, and then concentrated in vacuo. The residue was diluted with water (300 ml) and extracted with ether (3×500 ml). The ether extracts were washed with water and brine, dried with MgSO4 and concentrated in vacuo to yield the crude product. Distillation through a Vigreaux column gave 2-(1-methylethylthio)benzenamine: bp 94° (2.2-2.4 mm).
WORKUP
后处理
- additionWhen the addition
- temperaturethe reaction mixture was refluxed for 3 hours
- concentrationconcentrated in vacuo
- additionThe residue was diluted with water (300 ml)
- extractionextracted with ether (3×500 ml)
- washThe ether extracts were washed with water and brine
- dry with materialdried with MgSO4
- concentrationconcentrated in vacuo
- customto yield the crude product
- distillationDistillation through a Vigreaux column