Sodium Carbonate Decahydrate → HCID 15837866, compound
Reaction equation
[Br:1][C:2]1([C:5]([NH:7][CH2:8][C:9](=[O:11])[CH3:10])=O)[CH2:4][CH2:3]1.O.O.O.O.O.O.O.O.O.O.C(=O)([O-])[O-].[Na+].[Na+]>S(=O)(=O)(O)O>[Br:1][C:2]1([C:5]2[O:11][C:9]([CH3:10])=[CH:8][N:7]=2)[CH2:3][CH2:4]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
4.62 g of 1-bromo-N-(2-oxopropyl)-cyclopropane-1-carbamide is held at 60° C. in 35.47 ml of concentrated sulfuric acid for 30 minutes. The cooled reaction mixture is stirred into ice water and made basic in batches with sodium carbonate decahydrate. Then, it is extracted with ethyl acetate, dried on sodium sulfate, and concentrated by evaporation. Chromatography of the oily residue on silica gel with ethyl acetate/hexane yields 2.79 g of title compound 8 as a yellowish oil.
Workup
- customThe cooled reaction mixture
- extractionThen, it is extracted with ethyl acetate
- customdried on sodium sulfate
- concentrationconcentrated by evaporation
Sources & evidence
- ORD record
- ord-c1b4d8d270344a35803fb12efee2dd07
- Source dataset
- uspto-grants-2003_07
- Patent number
- US06600058B1
Reaction notes
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