Water → HCID 22501140, Verbindung

Temperatur

2.5 °C

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%).

1. additionwas added dropwise to the above solution
2. stirringThe solution was stirred at the same temperature for 1 hr
3. customto partition the solution
4. washThe organic layer was washed with saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. additionTo the obtained dark brown oil was added ether (50 ml)
8. stirringthe mixture was stirred thoroughly
9. waitleft at room temperature overnight
10. filtrationfiltered
11. washwashed with ether
12. customdried

ORD-Eintrag

ord-ed68b3042d2b47d18e325f75acc2a22c

Quelldatensatz

uspto-grants-2005_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06878831B2