反应详情

温度

-25 °C

To 1.418 g of pyrocatechol were added 1.917 g of methyl dichlorophosphate and 11 ml of acetonitrile. The mixture was cooled to -25° C. and 2.605 g of triethylamine was added dropwise at -25° C. to -20° C. with stirring. The dropping funnel was washed with 1 ml of acetonitrile and the washings were added to the mixture. After stirring at the same temperature for 10 minutes, the reaction mixture was allowed to return to 10° C. and then filtered. The filtration residue was washed with a 5-ml and 3-ml portion of acetonitrile. The filtrate and washings were concentrated under reduced pressure on a water bath at 15° C. to 20° C. to give 3.102 g of methyl o-phenylene phosphate as a slightly turbid oil.

1. washThe dropping funnel was washed with 1 ml of acetonitrile
2. additionthe washings were added to the mixture
3. stirringAfter stirring at the same temperature for 10 minutes
4. customto return to 10° C.
5. filtrationfiltered
6. washThe filtration residue was washed with a 5-ml and 3-ml portion of acetonitrile
7. concentrationThe filtrate and washings were concentrated under reduced pressure on a water bath at 15° C. to 20° C.