Nitrogen → HCID 14415807, compound
Reaction equation
C[O:2][C:3]1[C:13]2[S:12][C:11]3[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=3[CH2:9][C:8](=[O:18])[C:7]=2[CH:6]=[CH:5][CH:4]=1.Cl.N1C=CC=CC=1.N#N>>[OH:2][C:3]1[C:13]2[S:12][C:11]3[CH:14]=[CH:15][CH:16]=[CH:17][C:10]=3[CH2:9][C:8](=[O:18])[C:7]=2[CH:6]=[CH:5][CH:4]=1Participants
4
Procedure
6-Methoxy-11H-dibenzo[b,f]thiepin-10-one (1.54 g, 6 mmol) and pyridine hydrochloride (10 g) were heated for 2 hours at 200° C. with stirring and N2 atmosphere. The reaction was cooled down to room temperature and then triturated in water (200 ml) The pale green precipitate was filtered and dried overnight in a vacuum oven (50° C.) (1.40 g, 96%). 1HNMR (300 MHz, DMSO-d6): δH=4.20 (2H, s), 7.05–7.69 (7H, m), 10.56 (1H, s).
Workup
- customtriturated in water (200 ml) The pale green precipitate
- filtrationwas filtered
- customdried overnight in a vacuum oven (50° C.) (1.40 g, 96%)
Sources & evidence
- ORD record
- ord-d4095d2c905d42b8b4f46efcdbaeb48e
- Source dataset
- uspto-grants-2006_05
- Patent number
- US07049313B2
Reaction notes
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