HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21476266, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 21476257 | HCID 21476257 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21476266 | HCID 21476266 | — |
Reaction Steps
Methyl iodide (0.564 ml) was added to a mixture of intermediate 11 (2 g) and potassium carbonate (1.75 g) in dry DMF (8 ml) at 23° under nitrogen. After 4.5 h, the mixture was poured into water (100 ml) and extracted with EA (2×100 ml). The combined extracts were washed with water and saturated brine then dried and evaporated. The residue was chromatographed with hexane- EA (8:1 to 6:1 to 4:1) as eluent to give a 70:30 mixture of the title compound with N-adamantan-1-yl-N-methylbenzene-1,2-diamine (904 mg) as a yellow solid, m.p. 68°-76° dec.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05686449 |
| Source dataset | uspto-grants-1997_11 |
| ORD ID | ord-2c94db15832e443aa33d405625748d8f |
| Source note | uspto-grants-1997_11 |