反应详情

温度

75 °C

A reaction mixture of 1,4,7-tris(tert-butoxycarbonylmethyl)-1,4,7,10-tetraaza-cyclododecane (7.57 g, 12.7 mmol), 2-chloro-N-(4-tert-butylphenylmethyl)-acetamide (3.60 g, 15 mmol) obtained from Example 2a and potassium carbonate (5.53 g, 40 mmol) in acetonitrile (100 ml) was heated to 75° C. and stirred under nitrogen-atmosphere overnight. The reaction mixture was cooled to room temperature and filtered. The filtrate was evaporated in vacuo and the residue was submitted to flash-chromatography (silica, MeOH/CHCl3). The fractions containing the product were combined and evaporated in vacuo resulting in the title compound being a yellow oil that crystallised upon storage.

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered
3. customThe filtrate was evaporated in vacuo
4. additionThe fractions containing the product
5. customevaporated in vacuo