Hydrochloric Acid → HCID 13902891, compound

0.69 g (3.7 mmol) of 5,5-dimethyl-2-(1-propynyl)-2-oxo-1,3,2-dioxaphosphorinane (III) was dissolved in 3 ml of acetonitrile, and 0.22 g (4.4 mmol) of hydrazine monohydrate was added thereto. The mixture was left for 30 hours at room temperature. Then, 4.8 g of 10% by weight hydrochloric acid was added thereto and stirred for one hour. The solvent was distilled off to about one-half of its initial volume under reduced pressure, and the reaction mixture diluted with 30 ml of 20% by weight sodium chloride aqueous solution, was extracted 2 times with 40 ml of chloroform. The chloroform layers were combined and dried over anhydrous sodium sulfate, followed by filtration. The solvent was distilled off to obtain 0.77 g (yield: about quantitative amount) of the desired product of 2-acetonyl-5,5-dimethyl-2-oxo-1,3,2-dioxaphosphorinane (IV) as colorless solid.

1. distillationThe solvent was distilled off to about one-half of its initial volume under reduced pressure
2. additionthe reaction mixture diluted with 30 ml of 20% by weight sodium chloride aqueous solution
3. extractionwas extracted 2 times with 40 ml of chloroform
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfollowed by filtration
6. distillationThe solvent was distilled off

ORD record

ord-c34b2d9df0dc437086e5fd16e23a2586

Source dataset

uspto-grants-1993_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05177237