Water → HCID 178505632, compound

Participants

Reaction Conditions

Reaction Steps

570 mg (5.535 mmol) of tert-butyl nitrite were dissolved in 20 ml of dry dimethylformamide, and 1000 mg (2.767 mmol) of the compound from example 53 suspended 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, 100 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 64:20:16→0:100:0). 10 mg of the title compound were obtained (1% of theory).

Provenance & Evidence