1,2-Dichloroethane → HCID 12150161, compound
Reaction equation
[C:1]1([N:7]2[C:11]3([CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[C:10](=[O:17])[NH:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:19]1[N:23]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[N:22]=[C:21]([CH3:30])[C:20]=1[CH:31]=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[Cl:47]CCCl>>[Cl:47][N:22]1[C:21]([CH2:30][N:14]2[CH2:13][CH2:12][C:11]3([N:7]([C:1]4[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=4)[CH2:8][NH:9][C:10]3=[O:17])[CH2:16][CH2:15]2)=[C:20]([CH3:31])[CH2:19][N:23]1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1Participants
5
Procedure
1-Phenyl-1,3,8-triazaspiro[4.5]decan-4-one (0.050 g, 0.216 mmol), 5-chloro-3-methyl-1-phenylpyrazole-4-carboxaldehyde (0.042 g, 0.216 mmol), and sodium triacetoxyborohydride (0.039 g, 0.216 mmol) were combined in dry 1,2-dichloroethane (10 mL). The reaction was stirred overnight at room temperature. The mixture was concentrated to about 1 mL and the residue was purified by preparative thin layer chromatography to yield the title compound as a white solid.
Workup
- concentrationThe mixture was concentrated to about 1 mL
- customthe residue was purified by preparative thin layer chromatography
Sources & evidence
- ORD record
- ord-aabf472fbd7041569a0cf514497767d8
- Source dataset
- uspto-grants-2006_05
- Patent number
- US07053101B2
Reaction notes
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