Reaction equation
[P:1](=[O:7])([NH2:6])([S:4][CH3:5])[O:2][CH3:3].[C:8](OC(=O)C)(=[O:10])[CH3:9]>S(OC)(OC)(=O)=O>[C:8]([NH:6][P:1](=[O:7])([S:4][CH3:5])[O:2][CH3:3])(=[O:10])[CH3:9]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
19.1 Grams of dimethyl sulfate were gradually added to 296 g (purity 86.3%) of O,O-dimethylphosphoramidothioate at 40° C. in 30 min and to the resultant were further added 1180 g of O,O-dimethyl phosphoramidothioate and 76.1 g of dimethyl sulfate at the same temperature over 2 hours separately. The resultant reaction mixture was further maintained at the temperature for 8 hours to obtain 1562 g of O,S-dimethyl phosphoramidothioate(purity: 79.1%). To 1562 g of obtained O,S-dimethyl phosphoramidothioate was added 1218 g of acetic anhydride and 41 g of dimethyl sulfate at 40° C. over an hour. The resultant was maintained at the temperature for an hour to complete the reaction to give 2799 g of crude O,S-dimethyl N-acetylphosphoramidothioate (purity: 49.13%).
Workup
- temperatureThe resultant was maintained at the temperature for an hour
- customthe reaction
Sources & evidence
- ORD record
- ord-843ac36d88e24a81a616fa73e09a94b1
- Source dataset
- uspto-grants-1997_11
- Patent number
- US05684174
Linked notes
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