HRID1483837
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 4-(1,3-dioxoisoindolin-2-yl)cyclohexane-1-sulfonamide (3 g, 9.7 mmol) and NH2NH2H2O (1 mL) in EtOH (15 mL) was heated at reflux for 30 min. After cooling, the pH was adjusted with diluted HCl to 5. The mixture was concentrated in vacuo. The residue was dissipated with 35% HCl (10 mL) and heating until all solid material was dissolved. Upon cooling, a crystalline material was filtered and the filtrated was concentrated to give crude 4-aminocyclohexane-1-sulfonamide (700 mg, 40%) as a yellow solid, which was used in the next step directly.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux for 30 min
- temperatureAfter cooling
- concentrationThe mixture was concentrated in vacuo
- temperatureheating until all solid material
- dissolutionwas dissolved
- temperatureUpon cooling
- filtrationa crystalline material was filtered
- concentrationthe filtrated was concentrated