Diisopropylamine → HCID 90039285, compound

Temperature

5 °C

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.

1. customThe flask was then closed tightly
2. temperatureslowly heated to 25° C
3. customwas formed
4. additionwas added to entire content of the flask
5. waitThen, after about 2 hours
6. additionwas added
7. customAfter the entire content of the flask reacted
8. washThe product of the reaction was then eluted on the column
9. additionfilled with silica gel with 200-mesh molecules
10. additiona mixture of solvents
11. customAs a result of the reaction

ORD record

ord-46c13f96118d480f99f30e513f896f8e

Source dataset

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09376460B2