Hydrochloric Acid → HCID 13902891, compound

Participants

Reaction Steps

A solution mixture of II and III obtained in Reference Example 1 was stirred under cooling with ice and 510 g (10.2 mol) of hydrazine monohydrate was dropwise added thereto. After the completion of dropwise addition, the solution mixture was stirred for 30 minutes (the reaction was completed in ten minutes), and 11.2 kg of 10% by weight hydrochloric acid was added thereto. The solution mixture was stirred for one hour at room temperature and 5.0 kg of the solvent was distilled off. The solution was subjected to salting-out by addition of 1.38 kg of sodium chloride and extracted 2 times with 15.8 kg of chloroform. The chloroform layers were combined and dried over anhydrous sodium sulfate, followed by filtration. The solvent was distilled off, and the residue was dissolved in 3.5 kg of toluene and cooled with ice. The crystal thus precipitated was collected by filtration by means of suction and washed with 1.0 kg of toluene cooled and dried to obtain 1,000 g (yield: 57.5% through 4 steps) of the desired product of 2-acetonyl-5,5-dimethyl-2-oxo-1,3,2-dioxaphosphorinane as colorless crystal.

Provenance & Evidence