Hydrochloric Acid → HCID 18536749, compound
Reaction equation
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:8]([O:12]CC)=[N:9]2)=[CH:4][C:3]=1[N:20]1[CH:24]=[C:23]([CH2:25][OH:26])[N:22]=[CH:21]1.Cl>C(O)C>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[C:8](=[O:12])[NH:9]2)=[CH:4][C:3]=1[N:20]1[CH:24]=[C:23]([CH2:25][OH:26])[N:22]=[CH:21]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
To a solution of the compound of Example 35 (740 mg, 1.97 mmol) in ethanol (50 ml) was added concentrated hydrochloric acid (5 ml), and the mixture was refluxed for 16 hours, attaching Dean-Stark refluxing apparatus equipped with molecular sieves 4A. After cooling, the precipitated crystals were collected by filtration, washed with ethanol and then dried under reduced pressure, thereby obtaining 994 mg of title compound as light brown powder. The yield was quantitative.
Workup
- temperaturethe mixture was refluxed for 16 hours
- temperaturerefluxing apparatus
- temperatureAfter cooling
- filtrationthe precipitated crystals were collected by filtration
- washwashed with ethanol
- customdried under reduced pressure
Sources & evidence
- ORD record
- ord-7195fb27b75c4498809eda286eb08427
- Source dataset
- uspto-grants-2003_05
- Patent number
- US06562839B1
Reaction notes
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