HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 66879628, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 66881586 | HCID 66881586 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66879628 | HCID 66879628 | 61% |
Reaction Steps
The compound (3.14 g, 15.2 mmol) obtained in step A was dissolved in N,N-dimethylformamide (30 ml), 60% sodium hydride (730 mg, 18.2 mmol) was added under ice-cooling with stirring, and thereafter the mixture was stirred at room temperature for 30 min. The reaction mixture was ice-cooled again, methyl iodide (1.9 ml, 30.4 mmol) was added with stirring, and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added water, and the precipitated solid was collected by filtration, washed with water, and dried under reduced pressure to give a bistered solid. Using this solid and according to the method of Reference Example 116, step B, the title compound (1.76 g, yield 61%) was obtained as a pale-bistered solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08513235B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-0f895cc325c140d6bb0df571cc5e46c1 |
| Source note | uspto-grants-2013_08 |