HRID1911084

反应详情

EQUATION

反应方程式

HRID 1911084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. stirringthe mixture was stirred for 2 h at 70° C
  2. extractionextracted 1× with water
  3. dry with materialThe organic phase was dried with MgSO4
  4. customevaporated down
  5. customThe residue was purified by chromatography (RP-HPLC-MS)
  6. customThe corresponding fractions were freeze-dried