Ammonia → HCID 178515461, compound
Reaction equation
C[O:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:7][C:8]3([C:16]4[N:17]=[CH:18][NH:19][CH:20]=4)[CH:13]([C:14]=2[CH:15]=1)[CH2:12][CH2:11][CH2:10][CH2:9]3.Br.N>O>[NH:19]1[CH:20]=[C:16]([C:8]23[CH2:7][C:6]4[CH:5]=[CH:4][C:3]([OH:2])=[CH:15][C:14]=4[CH:13]2[CH2:12][CH2:11][CH2:10][CH2:9]3)[N:17]=[CH:18]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
4-(3-Methoxy-4b,5,6,7,8,9-hexahydrofluoren-8a-yl)-1H-imidazole (0.042 g) was mixed with 48% HBr (2 ml) and refluxed for 2 hours. After cooling to the ambient temperature, water (2 ml) was added and the pH was adjusted to 10 with 25% NH3-solution. The precipitated crude product was filtered and washed with water (10 ml). Recrystallisation from methylene chloride/methanol (95:5) gave the pure product. The yield was 0.030 g.
Workup
- temperaturerefluxed for 2 hours
- additionwas added
- customThe precipitated crude product
- filtrationwas filtered
- washwashed with water (10 ml)
- customRecrystallisation from methylene chloride/methanol (95:5)
- customgave the pure product
Sources & evidence
- ORD record
- ord-6538d3edd133441794a5e5e6afee3d53
- Source dataset
- uspto-grants-2002_03
- Patent number
- US06362211B1
Reaction notes
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