HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 9799569, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 10665070 | HCID 10665070 | — |
| Product | HCID 9799569 | HCID 9799569 | — |
Reaction Steps
To a solution of 0.5 g of the product obtained in Step B in 20 ml of anhydrous dimethylformamide there are slowly added, at 0° C., under an inert atmosphere, 0.16 g of sodium hydride and then, after 15 minutes, 0.65 ml of dimethyl sulphate (6 equivalents). After 1 hour, the reaction mixture is hydrolysed using ice and is then extracted with ethyl acetate. After washing the organic phase with aqueous sodium hydroxide solution, it is dried over sodium sulphate and then evaporated in vacuo. Chromatography over silica gel (cyclohexane/acetone: 98/2) allows 0.42 g of the expected product to be obtained. Melting point: 188° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06642248B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-5f6fa2158dde48a69058e58af666f5fb |
| Source note | uspto-grants-2003_11 |