Water → HCID 54522201, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of 9 g of 1,3-dihydro-5-(2,6-dimethoxy-4-methylphenyl)-1-methyl-1,4-benzodiazepin-2-one in 300 ml of toluene are added portionwise, with cooling to -20° C., 7.8 g of potassium tert-butoxide, then the temperature is allowed to rise slowly to 0° C. over 35 minutes, the mixture is cooled to -20° C. and 3.9 g of isoamyl nitrite in 50 ml of toluene are added dropwise. The reaction mixture is then stirred at 0° C. for 90 minutes, followed successively by pouring of the reaction mixture into water, adjustment of the pH to 4 with acetic acid, extraction with ethyl acetate, washing of the organic phase with water, drying over sodium sulphate and evaporation to dryness. The residue is crystallized from isopropyl ether, filtered and dried to give beige crystals melting at 150° C.; Yield=76%.

Provenance & Evidence