Réaction #527475

Équation de réaction

product

1-(4-Aminophenyl)-3-acetyl-4-methyl-7,8-methylenedioxy-5H-2,3-benzodiazepine

calcium hydride

methyl isocyanate

→

aimed product

Rendement 82.4%

N1 -[4-(3-Acetyl-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepin-1-yl)-phenyl]-N3 -methylurea

Rendement 82.4%

Solvants

benzene

Conditions de réaction

Traitement

1. 1
   workup.ADDITIONwas added
2. 2
   AutreThe crystals formed
3. 3
   Filtrationafter coling were filtered
4. 4
   Lavagewashed with 3×3 ml of benzene
5. 5
   Autretriturated with 20 ml of hot benzene
6. 6
   FiltrationThe hot mixture was filtered
7. 7
   Lavagethe precipitate was washed with 3×3 ml of benzene
8. 8
   Autredried

Mode opératoire

0.70 g (2 mmol) of the product of Example 15 was dissolved in benzene dehydrated over calcium hydride, 0.3 ml (5 mmol) of methyl isocyanate was added and the reaction mixture was stirred at 50° C. for 4 hours. The crystals formed after coling were filtered, washed with 3×3 ml of benzene, then triturated with 20 ml of hot benzene. The hot mixture was filtered, the precipitate was washed with 3×3 ml of benzene and dried to give 0.65 g (79.6%) of the aimed product, m.p.: 168°-170° C. (decomp.).

Source