反应详情

A 19 mg-sample (0.07 mmol) of (tert-butyl)[(5-chloro-3-fluoro(2-thienyl))sulfonyl]amine was dissolved in neat TFA and stirred for 1 h, concentrated in vacuo and used directly in the next transformation. This sample was dissolved in 150 uL of DCM and 21 mg (0.084 mmol) of DSC was added followed by 21 μL (0.14 mmol) of DBU. This solution was stirred for 18 h, 26 mg (0.07) of 3-(4-aminophenyl)-1,3-dihydroquinazoline-2,4-dione trifluoroacetate salt was added plus 150 μL of dry acetonitrile and refluxed for 2 h. This material was then purified on RP-HPLC to afford 11 mg (34%) of the desired product. BS-MS: M+H+=495 (Cl).

1. concentrationconcentrated in vacuo
2. dissolutionThis sample was dissolved in 150 uL of DCM
3. addition21 mg (0.084 mmol) of DSC was added
4. stirringThis solution was stirred for 18 h
5. temperaturerefluxed for 2 h
6. customThis material was then purified on RP-HPLC