Реакция #323397

Уравнение реакции

pyrocatechol

methyl dichlorophosphate

acetonitrile

→

methyl o-phenylene phosphate

Выход 129.5%

Растворители

triethylamine

Условия реакции

Обработка

1. 1
   ПромывкаThe dropping funnel was washed with 1 ml of acetonitrile
2. 2
   workup.ADDITIONthe washings were added to the mixture
3. 3
   workup.STIRRINGAfter stirring at the same temperature for 10 minutes
4. 4
   Другоеto return to 10° C.
5. 5
   Фильтрацияfiltered
6. 6
   ПромывкаThe filtration residue was washed with a 5-ml and 3-ml portion of acetonitrile
7. 7
   КонцентрированиеThe filtrate and washings were concentrated under reduced pressure on a water bath at 15° C. to 20° C.

Методика

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.

Источник