HRID1911084
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
200 mg (1.7 mmol) cyclohexanediol was placed in 1.5 ml dimethylacetamide and 47 mg (1.17 mmol) sodium hydride (60%) were added and the mixture was stirred for 15 min at ambient temperature. Then 100 mg (0.31 mmol) 6.1 was added and the mixture was stirred for 2 h at 70° C. The reaction mixture was diluted with dichloromethane and extracted 1× with water. The organic phase was dried with MgSO4 and evaporated down. The residue was purified by chromatography (RP-HPLC-MS). The corresponding fractions were freeze-dried.
WORKUP
后处理
- stirringthe mixture was stirred for 2 h at 70° C
- extractionextracted 1× with water
- dry with materialThe organic phase was dried with MgSO4
- customevaporated down
- customThe residue was purified by chromatography (RP-HPLC-MS)
- customThe corresponding fractions were freeze-dried