Pyridine → HCID 19040320, compound

Temperature

20 °C

A solution 0.5 g (2.75 mmol) of 2-benzyloxy-1,3-propanediol in 3.0 mL of pyridine was stirred at 0° C. under N2 as 0.37 g (2.5 mmol) of methyl dichlorophosphate was added dropwise over 15 mins to keep the solution under 10° C. The cold bath was removed and the reaction mixture was stirred overnight at 20° C.(~14 h). The mixture was filtered, and washed with benzene (10 mL), and the filtrate was evaporated. The residue was dissolved in benzene: CH2Cl2 (1:1, 20 mL), washed with H2O (10 mL), saturated NaHCO3 (10 mL), saturated NaCl (10 mL) and dried over magnesium sulfate. Evaporation afforded 0.26 g (40%) of 5-benzyloxy-2-methyl-1,3,2-dioxaphosphorinane-2-oxide.

1. additionwas added dropwise over 15 mins
2. customunder 10° C
3. customThe cold bath was removed
4. filtrationThe mixture was filtered
5. washwashed with benzene (10 mL)
6. customthe filtrate was evaporated
7. dissolutionThe residue was dissolved in benzene: CH2Cl2 (1:1, 20 mL)
8. washwashed with H2O (10 mL), saturated NaHCO3 (10 mL), saturated NaCl (10 mL)
9. dry with materialdried over magnesium sulfate
10. customEvaporation

ORD record

ord-167fc66b442d41a0b72e85cb71e2dcb6

Source dataset

uspto-grants-1997_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05639732