Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Phosphorus oxychloride | HCID 24813 | — |
| Edukt | 2,2-Dimethyl-1-(2-naphthyl)-1,3-propanediol | HCID 22501147 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | HCID 22501140 | HCID 22501140 | 82,1% |
Reaktionsschritte
2,2-Dimethyl-1-(2-naphthyl)-1,3-propanediol (34.86 g, (0.151 mol) and triethylamine (42.9 g, 0.424 mol) were dissolved in dichloromethane (200 ml). Phosphorus oxychloride (24.3 g, 0.158 mol) dissolved in dichloromethane (50 ml) was added dropwise to the above solution under cooling to 1 to 4° C. with stirring for 1 hr 40 min. The solution was stirred at the same temperature for 1 hr, and water (60 ml) was added thereto to partition the solution. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. To the obtained dark brown oil was added ether (50 ml) and the mixture was stirred thoroughly and left at room temperature overnight. The solidified reaction product was pulverized, filtered, washed with ether and dried to give the title compound (38.62 g, yield 82.1%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US07420070B2 |
|---|
| Quelldatensatz | uspto-grants-2008_09 |
|---|
| ORD ID | ord-2e586959ce2c4594a713d6bfe57ed937 |
|---|
| Quellennotiz | uspto-grants-2008_09 |
|---|