Salicyl Alcohol → 2-Chloro-2H,4H-1,3,2lambda~5~-benzodioxaphosphinine-2-thione

温度

22 °C

Into a three-necked, 500 ml flask were placed 31 g (0.25 mole) o-hydroxybenzyl alcohol, 56 g (1.0 moles) calcium oxide, a catalytic amount (0.1 g) of acridine, and 600 ml of benzene. To this reaction mixture was added 46.5 g (0.275 mole) of thiophosphoryl trichloride, dropwise, over a period of 120 minutes with stirring. The temperature was maintained at 22° C by use of a water bath. After the addition of the thiophosphoryl trichloride the mixture was stirred overnight. The mixture was then filtered, the solids washed with four equal portions of benzene (total of 200 ml) and the washings combined with the filtrate. The filtrate was then washed with two equal portions of a 5 percent aqueous bicarbonate solution (total of 100 ml), dried over sodium sulfate, filtered, and the volatiles removed under reduced pressure. The residue crystallized, affording 39 g (71%) pf 2-chloro-4H-1,3,2-benzodioxaphosphorin-2-sulfide, m.p.=44°-45° C. Analysis: %Cl, 16.12 (calculated); 16.42 (Found).

1. customInto a three-necked, 500 ml flask were placed
2. stirringwas stirred overnight
3. filtrationThe mixture was then filtered
4. washthe solids washed with four equal portions of benzene (total of 200 ml)
5. washThe filtrate was then washed with two equal portions of a 5 percent aqueous bicarbonate solution (total of 100 ml)
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. customthe volatiles removed under reduced pressure
9. customThe residue crystallized

ORDレコード

ord-b9625f5a5c254fd3bba1a0d558b822b0

出典データセット

uspto-grants-1978_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04087490