HCID 58959693, compound → HCID 58959701, compound
Reaction equation
C[O:2][C:3]([C:5]1[C:6]2[C:7](=[O:21])[CH:8]=[C:9]([C:16]([O:18]CC)=[O:17])[NH:10][C:11]=2[C:12]([F:15])=[CH:13][CH:14]=1)=[O:4]>Cl>[F:15][C:12]1[C:11]2[NH:10][C:9]([C:16]([OH:18])=[O:17])=[CH:8][C:7](=[O:21])[C:6]=2[C:5]([C:3]([OH:4])=[O:2])=[CH:14][CH:13]=1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 100 °C
Procedure
To a 2 N aqueous HCl (200 mL) solution was added 34 (10.0 g, 34.1 mmol). The reaction mixture was heated at 100° C. for 18 h and then cooled to room temperature. The resulting precipitate was filtered and dried under vacuum at 60° C. for 18 h to afford an off-white solid (35, 8.11 g, 94.7%). 1H NMR (DMSO-d6, 300 MHz) δ ?7.65 (t, J=8.2, 1H), 7.39-7.43 (m, 1H), 6.93 (s, 1H).
Workup
- temperaturecooled to room temperature
- filtrationThe resulting precipitate was filtered
- customdried under vacuum at 60° C. for 18 h
- customto afford an off-white solid (35, 8.11 g, 94.7%)
Sources & evidence
- ORD record
- ord-8d52047dd96b476d93df148e8151993e
- Source dataset
- uspto-grants-2008_11
- Patent number
- US07456178B2
Reaction notes
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