Reaction equation
S(O)(O)(=O)=O.[CH3:6][O:7][C:8](=[NH:10])[NH2:9].[CH3:11][O:12][C:13](Cl)=[O:14].[OH-].[Na+]>O>[CH3:11][O:12][C:13]([NH:10][C:8](=[NH:9])[O:7][CH3:6])=[O:14]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
246 g of O-methylisourea sulfate are dissolved in 300 ml of water and 163 ml of chloroformic acid methyl ester are added dropwise at 10° C., followed by 170 g of NaOH, dissolved in 510 ml of water. The mixture is stirred at room temperature for a further 3 hours. The reaction solution is then extracted with ethyl acetate and this extract is dried with anhydrous sodium sulfate. Evaporation under reduced pressure at a maximum bath temperature of 40° C. gives the N-methoxycarbonyl-O-methylisourea as an oil, which gradually solidifies to form crystals with a melting point of 40° C. Yield 150 g.
Workup
- extractionThe reaction solution is then extracted with ethyl acetate
- dry with materialthis extract is dried with anhydrous sodium sulfate
- customEvaporation under reduced pressure at a maximum bath temperature of 40° C.
Sources & evidence
- ORD record
- ord-6b9117b65bf24eb2a443470fd78e9f40
- Source dataset
- uspto-grants-1981_03
- Patent number
- US04254143
Linked notes
Loading…