Diisopropylamine → HCID 90039285, compound

Participants

Reaction Conditions

Reaction Steps

50 mL of anhydrous benzene was placed in a flask under argon. The flask was then closed tightly, followed by an addition of a freshly distilled phosphoric chloride (III) (876λ 1; 10 mmole). The flask was then cooled down to a temperature of 5° C., and the anhydrous N,N-diisopropylamine (7.7 ml; 55 mmole) was added. The reaction mixture was stirred for 30 minutes, and then slowly heated to 25° C. The temperature was then maintained until the bis(N,N-diisopropylamine) chlorophosphite was formed. After the reaction was completed in 98% (about 3 days), 2-(2-pyridyl)aminoethanol (1.38 mg; 10 mmole) was added to entire content of the flask. Then, after about 2 hours, 1-H-tetrazole (700 mg; 10 mmole) dissolved in anhydrous benzene (5 mL) was added. After the entire content of the flask reacted, 1 μl of diisopropylamine was added. The product of the reaction was then eluted on the column filled with silica gel with 200-mesh molecules. The eluent phase used a mixture of solvents: benzene and triethylamine, with a benzene volume fraction of 90%. As a result of the reaction, 2-isopropyl-3-(pyrid-2-yl)-[1,3,2]oxazaphospholidine was obtained.

Provenance & Evidence