Hydrochloric Acid → HCID 9939091, compound
Reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]2[C:13]([C:14]([O:16]CCC#N)=[O:15])=[C:12]([CH3:21])[NH:11][C:10]([CH2:22][O:23][CH2:24][CH2:25][CH:26]3[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]3)=[C:9]2[C:32]([O-])=[O:33])[CH:5]=[CH:6][CH:7]=1.CCN=C=NCCCN(C)C.Cl.[C:47]1([CH:53]([C:57]2[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=2)[CH2:54][CH2:55][NH2:56])[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1.Cl>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]2[C:9]([C:32](=[O:33])[NH:56][CH2:55][CH2:54][CH:53]([C:47]3[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=3)[C:57]3[CH:62]=[CH:61][CH:60]=[CH:59][CH:58]=3)=[C:10]([CH2:22][O:23][CH2:24][CH2:25][CH:26]3[CH2:27][CH2:28][CH2:29][CH2:30][CH2:31]3)[NH:11][C:12]([CH3:21])=[C:13]2[C:14]([OH:16])=[O:15])[CH:5]=[CH:6][CH:7]=1Participants
6
Procedure
0.25 g (0.51 mmol) of 5-(2-cyanoethyl) 4-(3-chlorophenyl)-2-(2-cyclohexylethoxymethyl)-6-methyl-1,4-dihydropyridine-3,5-dicarboxylate, 0.12 g (0.63 mmol) of WSC hydrochloride and 0.13 g (0.62 mmol) of 3,3-diphenylpropylamine were stirred together in 5 ml of dichloromethane at room temperature for 16 hours. 0.1 N hydrochloric acid was added to the reaction mixture. After the extraction with dichloromethane, the organic layer was concentrated under reduced pressure. The residue was purified by the silica gel chromatography (hexane/ethyl acetate=1/1) to obtain the title compound.
Workup
- extractionAfter the extraction with dichloromethane
- concentrationthe organic layer was concentrated under reduced pressure
- customThe residue was purified by the silica gel chromatography (hexane/ethyl acetate=1/1)
Sources & evidence
- ORD record
- ord-2a14f2f9c6a84ce39c2c730153290f63
- Source dataset
- uspto-grants-2003_08
- Patent number
- US06610717B2
Reaction notes
Loading…