Methanol → HCID 21453530, Verbindung

Into a 3-necked flask fitted with a stirrer, thermometer and drying tube, a solution of 91.8 g. (0.6 mole) POCl3 and 127 g. (0.6 mole) 2,4,4,4-tetrachlorobutanol in a mixture of 400 mls. of carbon tetrachloride and 100 mls. of chloroform was poured. A total of 52 g. (0.67 mole) of pyridine was added dropwise while stirring and holding the temperature below 12° C. A mixture of 42 g. (1.3 moles) of methanol in 104 g. (1.3 moles) of pyridine was added while keeping the temperature below 21° C. After completion of the reaction the organic phase was successively washed with aqueous 20% H2SO4 solution, water, saturated aqueous NaHCO3, and water. The solution was dried and concentrated at reduced pressure to give 158 g. (82%) of dimethyl-2,4,4,4-tetrachlorobutyl phosphate. Distillation at 130° C./0.3 mm. gave a purified product having n(24/D) 1.4766. The phosphate structure was substantiated by infrared analysis. Elemental Analysis: Calcd. for C6H11Cl4O4P: percent Cl, 44.38; percent P, 9.69 Found: percent Cl, 45.49; percent P, 9.48.

1. customInto a 3-necked flask fitted with a stirrer
2. customthermometer and drying tube
3. customthe temperature below 12° C
4. additionA mixture of 42 g
5. customthe temperature below 21° C
6. customAfter completion of the reaction the organic phase
7. washwas successively washed with aqueous 20% H2SO4 solution, water, saturated aqueous NaHCO3, and water
8. customThe solution was dried
9. concentrationconcentrated at reduced pressure
10. customto give 158 g
11. distillationDistillation at 130° C./0.3 mm
12. customgave a purified product

ORD-Eintrag

ord-51f7eb8d34cd4cba89cf711cca32a19e

Quelldatensatz

uspto-grants-1977_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04008187