2-CHLORO-5 5-DIMETHYL-1 3 2-DIOXAPHOSPHO synthesis
- Product Name:2-CHLORO-5 5-DIMETHYL-1 3 2-DIOXAPHOSPHO
- CAS Number:2428-06-0
- Molecular formula:C5H10ClO2P
- Molecular Weight:168.56
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2428-06-0
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Yield: 95%
Reaction Conditions:
with anhydrous phosphorus trichloride in toluene
Steps:
1 EXAMPLE 1
EXAMPLE 1 Phosphorus trichloride (1.25 mol) is added over a period of 90 minutes to a solution of neopentyl glycol (1.25 mol) in 750 mL of toluene at 0°C. The reaction mixture is stirred at 0 to 5°C for an additional 60 minutes and then is heated to 90°C and 2-(1,1-dimethylethyl)-4-methoxyphenol (0.625 mol) is added over 10 to 15 minutes. The reaction is heated to and held at reflux for 30 minutes and toluene is removed to a head temperature of 110°C. The mixture is held at 110°C for 4 hours with nitrogen sparging. The remaining toluene is removed to 120°C head temperature and 170°C pot temperature. Excess 2-chloro-5,5-dimethyl-1,3,2,- dioxaphosphorinane is removed at 125°C head temperature under a vacuum of 10 mm. (FDMS MW=168) The product, 2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane, is collected by distillation at 9 mm and 198°C head temperature. It is obtained in a yield of 95% and a purity of 100% by gas chromatography analysis. FDMS MW=312; Viscosity: 500+-5 cps at 27°C.
References:
EASTMAN KODAK COMPANY EP382660, 1990, A1
126-30-7
624 suppliers
$8.00/100g
2428-06-0
29 suppliers
$191.00/25g
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1000210-73-0
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2428-06-0
29 suppliers
$191.00/25g