Sodium hydride → HCID 15678607, compound

Participants

Reaction Steps

To a suspension of NaH (70 mg of NaH was washed with hexane several times dispersed in 50% mineral oil) in 4ml of DNF is added a solution of 1,3-dihydro-5-phenyl-1-methyl-2H-1,3,4-benzotriazepine-2-one (251 mg) in 5 ml DMP under nitrogen atmosphere. After gas evolution ceased, 0.13 ml 4-fluorobenzoyl chloride is added and the mixture is stirred at room temperature overnight (about 12-6 hours). Solvent is removed in vacuo to a dryness and the residue is partitioned between ethylacetate and water. Organic layer is washed with aq.NaHCO3, water, then dried over MgSO4. After evaporation of solvent, the residue is recrystallized using methanol as a solvent. About 97mg of a product is obtained. TLC: (Silica gel - Chloroform/acetone=9:1, Rf.=0.52).

Provenance & Evidence