5,11-dihydro-11-[(4-methoxy-phenyl)-methyl]-5-methyl-6H-dipyrido-[3,2-b:2',3'-e][1,4]diazepin-6-one → 5,11-dihydro-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one
Reaction equation
COC1C=CC(C[N:10]2[C:16]3[N:17]=[CH:18][CH:19]=[CH:20][C:15]=3[C:14](=[O:21])[N:13]([CH3:22])[C:12]3[CH:23]=[CH:24][CH:25]=[N:26][C:11]2=3)=CC=1>FC(F)(F)C(O)=O>[CH3:22][N:13]1[C:14](=[O:21])[C:15]2[CH:20]=[CH:19][CH:18]=[N:17][C:16]=2[NH:10][C:11]2[N:26]=[CH:25][CH:24]=[CH:23][C:12]1=2Participants
3
Procedure
50 ml of trifluoroacetic acid was added to 10.3 g (0.030 mol) of 5,11-dihydro-11-[(4-methoxyphenyl)methyl]-5-methyl-6H-dipyrido [3,2-b:2',3'-e][1,4]-diazepin-6-one, and the mixture was stirred for one hour at room temperature. The acid was removed in vacuo and the residue was stirred for one hour with 0.5% ammonia. The solid was filtered and dried to give 6.70 g (98% of theory) of pure 5,11-dihydro-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one, m.p. 230°-232° C.
Workup
- customThe acid was removed in vacuo
- stirringthe residue was stirred for one hour with 0.5% ammonia
- filtrationThe solid was filtered
- customdried
Sources & evidence
- ORD record
- ord-2c7e5a2a0f0a4ea7860b29d45555a7a3
- Source dataset
- uspto-grants-1994_11
- Patent number
- US05366972
Reaction notes
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