Diethyl Ether → HCID 66938706, compound
Reaction equation
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([N:10]([CH3:38])[C:11](=[O:37])[CH2:12][N:13]([C:24]2[CH:29]=[C:28]([C:30]3[N:34]=[C:33]([CH3:35])[O:32][N:31]=3)[CH:27]=[CH:26][C:25]=2[CH3:36])[CH2:14][C:15]([NH:17][CH2:18][CH2:19][NH:20][CH:21]([CH3:23])[CH3:22])=[O:16])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[ClH:39].C(OCC)(=O)C.C(OCC)C>C(OCC)(=O)C>[ClH:39].[C:1]([N:4]1[CH2:5][CH2:6][CH:7]([N:10]([CH3:38])[C:11](=[O:37])[CH2:12][N:13]([C:24]2[CH:29]=[C:28]([C:30]3[N:34]=[C:33]([CH3:35])[O:32][N:31]=3)[CH:27]=[CH:26][C:25]=2[CH3:36])[CH2:14][C:15]([NH:17][CH2:18][CH2:19][NH:20][CH:21]([CH3:23])[CH3:22])=[O:16])[CH2:8][CH2:9]1)(=[O:3])[CH3:2]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
The compound (161 mg, 0.303 mmol) obtained in step E was dissolved in ethyl acetate (2 ml), 4N hydrochloric acid-ethyl acetate solution (0.16 ml) was added at room temperature with stirring, and the mixture was stirred at the same temperature for 2.5 hr. To the reaction mixture was added diethyl ether (2 ml), the precipitated solid was collected by filtration, washed with diethyl ether, and dried under reduced pressure to give the title compound (164 mg, yield 96%) as a colorless solid.
Workup
- stirringthe mixture was stirred at the same temperature for 2.5 hr
- filtrationthe precipitated solid was collected by filtration
- washwashed with diethyl ether
- customdried under reduced pressure
Sources & evidence
- ORD record
- ord-170c720219fe401fa6e67e9ce6707603
- Source dataset
- uspto-grants-2013_08
- Patent number
- US08513235B2
Reaction notes
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