HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → 1-Methyl-3-(1-methylethyl)-pyrido(2,3-c)(1,2,6)-thiadiazin-4(3H)-one-2,2-dioxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3-(1-Methylethyl)pyrido(2,3-c) (1,2,6)thiadiazin-4(3H)-one-2,2-dioxide | HCID 13609243 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Product | 1-Methyl-3-(1-methylethyl)-pyrido(2,3-c)(1,2,6)-thiadiazin-4(3H)-one-2,2-dioxide | HCID 22756783 | — |
Reaction Steps
3-(1-Methylethyl)pyrido(2,3-c)(1,2,6)thiadiazin-4(3H)-one-2,2-dioxide (5.0 grams; 0.0208 mole) was mixed with 50 ml of diethylene glycol dimethyl ether. The system was flushed with nitrogen and sodium hydride (1.0 gram; 0.02 mole), previously washed with n-hexane, was added portionwise to the reaction mixture. After the effervescence of hydrogen ceased, 2.2 ml of dimethyl sulfate (0.023 mole, 1.33g/ml) was added and the reaction mixture heated at reflux temperatures for a period of 4 hours. During the reaction, the color of the reaction mixture changed from light yellow to deep red and gradually back to yellow.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04129734 |
| Source dataset | uspto-grants-1978_12 |
| ORD ID | ord-d52400201d5a4605b8eda72520164e2c |
| Source note | uspto-grants-1978_12 |