HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → HCID 20138881, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | 7-Methoxy-1,2,3,4-tetrahydronaphthalen-1-one | HCID 81276 | — |
| Catalyst | Titanium | HCID 23963 | — |
| Catalyst | Titanium Tetrachloride | HCID 24193 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 20138881 | HCID 20138881 | 87.5% |
Reaction Steps
A solution of titanium tetrachloride (53.8 g, 31.2 ml) in dry toluene (200 ml) is added over a period of 45 minutes to a stirred solution of 7-methoxy-1-tetralone (100.5 g) and dimethyl amine (171 g) in dry toluene (2 l) while maintaining a reaction temperature of ≤10° C. When the addition of the titanium is complete, the ice bath is removed and the solution allowed to reach RT. The solution is stirred at RT for 3 hours. The solids are filtered, washed with dry toluene and the filtrate evaporated in vacuo, yielding 101.4 g of an amber oil which is used in the next step without further treatment.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04588719 |
| Source dataset | uspto-grants-1986_05 |
| ORD ID | ord-032e3c2be01c4129889814826fa7ebd1 |
| Source note | uspto-grants-1986_05 |