反应详情

To crude 5-chloro-N,N-bis((2-(trimethylsilyl)ethoxy)methyl)pyrazolo[1,5-a]pyrimidin-7-amine (Int-9d, 7.9 g) (prepared as described in Steps A-D of Example 9) in CH3CN (100 mL) was added N-iodosuccinimide (4.3 g, 19.2 mmol) and the resulting mixture was stirred at room temperature for 30 mins, at which time LC/MS confirmed full conversion of starting material to product. Saturated sodium thiosulfate solution (˜20 mL) was added and stirring continued for 5 minutes before the mixture was transferred to a separatory funnel using CH2Cl2 (30 mL) and H2O (30 mL). Brine (50 mL) was added and organics were extracted with CH2Cl2 (4×40 mL), dried (Na2SO4) and concentrated in vacuo to give crude 5-chloro-3-iodo-N,N-bis((2-(trimethylsilyl)ethoxy)methyl)pyrazolo[1,5-a]pyrimidin-7-amine (Int-10a) as a light brown liquid (10.4 g). LCMS: 2.95 mins, m/z=555.1 (MH+).

1. stirringstirring
2. waitcontinued for 5 minutes before the mixture
3. customwas transferred to a separatory funnel
4. extractionorganics were extracted with CH2Cl2 (4×40 mL)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo