تفاعل #53361

معادلة التفاعل

starting material XXIV

(±)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbamidoxime

triethyl orthoformate

hydrochloric acid

→

title compound

المردود 75.0%

(±)-8-Methyl-5-(4-nitrophenyl)-7-(1,2,4-oxadiazol-3-yl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

المردود 75.0%

ظروف التفاعل

المعالجة

1. 1
   تركيزconcentrated in vacuum
2. 2
   workup.STIRRINGThe residue was stirred with water
3. 3
   ترشيحthe precipitated crystals were filtered off
4. 4
   غسيلwashed with water
5. 5
   أخرىrecrystallized from 2-methoxyethanol

الإجراء التجريبي

A mixture of 1.50 g (3.91 mmol) of the starting material XXIV and 15 ml of triethyl orthoformate in the presence of 0.05 ml of 36% hydrochloric acid was stirred at 110° C. for 30 min, then concentrated in vacuum. The residue was stirred with water, the precipitated crystals were filtered off, washed with water and recrystallized from 2-methoxyethanol to yield 1.15 g (75%) of the title compound; Mp.: 190-196° C.

المصدر