Morpholine → HCID 22566227, compound
Reaction equation
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:14][CH2:13][CH2:12][C:11](Cl)(Cl)[CH2:10][C:9]2=[O:17])=[C:4]([F:18])[CH:3]=1.[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:14][CH2:13][CH2:12][CH:11]=[C:10]([N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)[C:9]2=[O:17])=[C:4]([F:18])[CH:3]=1Participants
3
Procedure
N-[4-bromo-2-fluorophenyl]-3,3-dichlorocaprolactam (0.49 g, 1.38 mmol) was refluxed with 10 mL of morpholine under N2 for 1 h. The solvent was then removed in vacuo. Toluene was added and the solid was filtered off. The filtrate was concentrated and dried under vacuum to give 1,5,6,7-tetrahydro-1-[4-bromo-2-fluorophenyl]-3-(morpholin-4-yl)-2H-azepin-2-one as brown oil(0.55 g). LRMS (AP+): 369.0, 371.0, (M+H)+.
Workup
- customThe solvent was then removed in vacuo
- additionToluene was added
- filtrationthe solid was filtered off
- concentrationThe filtrate was concentrated
- customdried under vacuum
Sources & evidence
- ORD record
- ord-f74fae152c064e04a1a485cb4e0a3d77
- Source dataset
- uspto-grants-2002_07
- Patent number
- US06413980B1
Reaction notes
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