Acetic Acid → Ethyl 1-methyl-2-cyanoethyl(diethoxymethyl)phosphinate

The starting material may be prepared as follows: A solution of 23.5 g of ethyl (diethoxymethyl)phosphonite and 6.7 g of crotononitrile in 30 ml of dry ethanol is added to a stirred mixture of 1.2 g of sodium hydride (50% dispersion in oil) in 30 ml of ethanol at 0° C. under an atmosphere of nitrogen. The reaction mixture is allowed to warm to room temperature and stirred for 4 hours. 1 ml of glacial acetic acid is added and the mixture concentrated under reduced pressure. The resulting crude product is dissolved in 50 ml of ethyl acetate, washed twice with 25 ml of water, and the organic extract is dried over magnesium sulphate, and then concentrated under reduced pressure. The crude product is distilled under reduced pressure to give ethyl 2-cyano-1-methylethyl(diethoxymethyl)phosphinate, b.p. 116° C./0.01 mbar, 31P=+42.2 and +42.0 ppm (CDCl3).

1. customThe starting material may be prepared
2. concentrationthe mixture concentrated under reduced pressure
3. dissolutionThe resulting crude product is dissolved in 50 ml of ethyl acetate
4. washwashed twice with 25 ml of water
5. extractionthe organic extract
6. dry with materialis dried over magnesium sulphate
7. concentrationconcentrated under reduced pressure
8. distillationThe crude product is distilled under reduced pressure

ORD 기록

ord-803295e0f1674a0cb8723312c57ccc26

출처 데이터셋

uspto-grants-1987_04

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04656298