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ChemicalBook CAS DataBase List 1,3,2-Dioxaphospholane, 2-methoxy-, 2-oxide
2196-04-5

1,3,2-Dioxaphospholane, 2-methoxy-, 2-oxide synthesis

5synthesis methods
-

Yield:2196-04-5 95%

Reaction Conditions:

in dichloromethane at 0 - 20; for 12 h;

Steps:

21 Example 21Preparation of compound 21 (vinyl methyl phosphate or 2-methyl-2-oxo-1,3,2-dioxaphosphalane):

Add 200 g of dichloromethane and 42 g of methanol (reactant C) to a 500 ml three-necked flask at room temperature, and stir for 0.5 h at room temperature. The solution is colorless and transparent. The three-necked flask is connected to an external gas absorption device, and then 143 g of the reaction intermediate B is dropped through The liquid funnel was slowly added to a 500ml three-necked flask, the dropping rate was controlled to 1 drop / second, and the reaction temperature was 0 ° C. With the addition of the reaction intermediate B, a large amount of heat was released and a large amount of HCl gas was released. The solution was colorless and transparent. Stirring was continued for 12 h at room temperature, and then dichloromethane was removed to obtain a pale yellow liquid. The pale yellow liquid was distilled under reduced pressure at 100 ° C to obtain 131 g of a colorless and transparent liquid with a yield of 95%. This product is compound 21 (vinyl methyl phosphate or 2-methyl-2-oxo-1,3,2-dioxocyclopentane).The HCl gas generated by the reaction is absorbed by water to obtain hydrochloric acid. The hydrochloric acid is sold as a chemical raw material. The organic solvent used in the reaction is distilled and dried to be recovered and reused.

References:

CN110590848,2019,A Location in patent:Paragraph 0146-0149