Tributyl phosphite → Ethyl 2-dibutoxyphosphorylacetate

Temperature

120 °C

100 parts by weight of tributyl phosphite and 66 parts by weight of ethyl bromoacetate were put into a reactor equipped with a distillation tube, and the inside of the reactor was substituted by nitrogen. Subsequently, the reactor was heated at 120° C. to start a reaction. Since bromobutane as a by-product began to distill out immediately, the reaction was maintained until the distillation-out of bromoethane slowed down. When the distillation-out of bromoethane became moderate, the reactor was further heated at 170° C. to continue the reaction for 3 hours. The reaction mixture was distilled at 180° C. under a reduced pressure to obtain an achromatic transparent liquid (yield of 88%, boiling point of 249° C./760 mmHg).

1. customequipped with a distillation tube
2. customa reaction
3. distillationto distill out immediately
4. temperaturethe reaction was maintained until the distillation-out of bromoethane
5. distillationWhen the distillation-out of bromoethane
6. temperaturethe reactor was further heated at 170° C.
7. customthe reaction for 3 hours
8. distillationThe reaction mixture was distilled at 180° C. under a reduced pressure
9. customto obtain an achromatic transparent liquid (yield of 88%, boiling point of 249° C./760 mmHg)

ORD record

ord-68b44a75830f4a3d9e5b60691937364b

Source dataset

uspto-grants-2012_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08263690B2