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
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
A small screw cap test tube was charged with 5-Acetyl-thiophene-2-carboxylic acid [3-(3-hydroxymethylene-2-oxo-2,3-dihydro-1H-indole-6-carbonyl)-phenyl]-amide (as prepared in Example 54, 100 mg, 0.231 mmol) and THF (2 mL). To the resulting solution was added N-(4-aminophenyl)morpholine (45.34 mg, 0.254 mmol), and the mixture was stirred for 24 h at 65° C. Subsequently, the reaction mixture was cooled to room temperature. Hexanes (5 mL) were added to the reaction mixture. The crude mixture was concentrated in vacuo and then dissolved into hot EtOAc. Hexanes (˜5 mL) were added causing a precipitate to crash out. The precipitate was filtered and washed with ˜1 mL of i-prOH yielding 69% (95 mg, 0.160 mmol) of the title compound.
WORKUP
后处理
- customA small screw cap test tube
- temperatureSubsequently, the reaction mixture was cooled to room temperature
- concentrationThe crude mixture was concentrated in vacuo
- dissolutiondissolved into hot EtOAc
- additionHexanes (˜5 mL) were added
- filtrationThe precipitate was filtered