Ammonia → HCID 13828992, compound

Participants

Reaction Conditions

Reaction Steps

14.2 g (78.0 mmol) of 30 were suspended in 175 ml of pyridine in a 250 ml three-necked flask equipped with an internal thermometer and reflux condenser and the mixture was treated with 61.4 g (234 mmol) of triphenylphosphine2). It was heated at 60° C. for 5 hours and stirred overnight at room temp. (TLC checking, CHCl3/MeOH 5:1). 40 ml of 25% strength ammonia solution were added to the suspension, which then clarified. The solvents were removed in vacuo in a rotary evaporator. The residue was stirred at room temp. for 30 min in 200 ml of CH2Cl2/MeOH 1:1, and the recipitate was filtered off and washed with CH2Cl2. After drying in vacuo in a desiccator over phosphorus entoxide, 10.0 g (85%) of 31 of m.p. 214-220° C. were obtained.

Provenance & Evidence