HRID536556
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
An amount of 50 mg (0.11 mmol) of the compound from Example 28A was introduced in 1 ml of DMF and admixed with 18 mg (0.14 mmol) of HOBt and with 28 mg (0.15 mmol) of EDC. After 10 minutes of stirring at RT, 13 μl (0.12 mmol) of 2-methylpropan-2-amine were added and the mixture was stirred at room temperature for 16 h. Subsequently the reaction solution was admixed with about 3 ml of water and extracted with twice 5 ml of ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated under reduced pressure. The crude product was purified by chromatography [Method 8]. This gave 31 mg (55% of theory) of the target compound.
WORKUP
后处理
- stirringthe mixture was stirred at room temperature for 16 h
- extractionextracted with twice 5 ml of ethyl acetate
- dry with materialThe combined organic phases were dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe crude product was purified by chromatography [Method 8]