Water → HCID 66614084, compound

Participants

Reaction Conditions

Reaction Steps

447 mg (4.337 mmol) of tert-butyl nitrite were dissolved in 20 ml of dry dimethylformamide, and 994 mg (2.169 mmol) of the compound from example 44 dissolved in 15 ml of dimethylformamide were added at 65° C. by means of a syringe pump within 1 h. After stirring at 65° C. for a further hour, 40 ml of water were added, forming a precipitate. The precipitate was filtered off and purified by means of preparative HPLC (eluent: water/acetonitrile/water with 1% trifluoroacetic acid, gradient 68:15:17→0:100:0). 99 mg of the title compound were obtained (10% of theory).

Provenance & Evidence