反应详情

温度

65 °C

Zn dust (1.80 g, 27.5 mmol) was vigorously stirred in DMA (11 ml) under nitrogen and the suspension was heated at 65° C. Trimethylsilyl chloride (0.37 g, 3.39 mmol) and 1,2-dibromoethane (0.64 g, 3.39 mmol) was added and stirring continued for 40 min. A solution of 3-iodo-azetidine-1-carboxylic acid tert-butyl ester (6.00 g, 21.2 mmol) in dimethylacetamide (DMA, 10 ml) was then added dropwise to the solution over a period of 30 min and then the reaction mixture allowed to cool to room temperature over 16 h. The resulting solution was used without any purification in the next step.

1. temperatureto cool to room temperature over 16 h
2. customThe resulting solution was used without any purification in the next step