Sodium Bicarbonate → HCID 14883431, compound
Reaction equation
[N:1]1[CH:6]=[CH:5][C:4]([C:7]([NH:9][N:10]([CH3:15])[C:11]([NH:13][CH3:14])=[S:12])=O)=[CH:3][CH:2]=1.C([O-])(O)=O.[Na+]>>[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[N:13]([CH3:14])[C:11](=[S:12])[N:10]([CH3:15])[N:9]=2)=[CH:3][CH:2]=1Participants
3
Procedure
The 1:1 mixture from Example 2 and 1 molar aqueous NaHCO3 (100 ml, 1.00×10-1 mole) were stirred and warmed to reflux. After refluxing for 15 hours the reaction was allowed to cool in an ice bath. The resulting precipitate was collected by filtration and was dried by suction. The desired product was crystallized from ethyl acetate/hexane to yield large colorless plates: 4.1 g (35%), mp 150°-152° C.
Workup
- temperaturewarmed to reflux
- temperatureAfter refluxing for 15 hours the reaction
- temperatureto cool in an ice bath
- filtrationThe resulting precipitate was collected by filtration
- customwas dried by suction
- customThe desired product was crystallized from ethyl acetate/hexane
- customto yield large colorless plates
Sources & evidence
- ORD record
- ord-db7f6b9004554351a799a41079d7f70f
- Source dataset
- uspto-grants-1990_08
- Patent number
- US04952593
Reaction notes
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