Bromotrimethylsilane → HCID 20337186, compound

Participants

Reaction Steps

A mixture of dimethyl 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-trans-1-propenylphosphonate (3.70 g.) and trimethylbromosilane (8.71 g.) was stirred for 30 minutes under ice-cooling and for 30 minutes at ambient temperature. Subsequently, the reaction mixture was concentrated under reduced pressure to give a residue. To the residue was added water (25 ml.). After the mixture was stirred for an hour at ambient temperature, the mixture was washed three times with chloroform (10 ml.), and then concentrated under reduced pressure to give oily 3-(N-ethoxycarbonyl-N-ethoxycarbonyloxyamino)-trans-1-propenylphosphonic acid (2.80 g.). Furthermore, the combined chloroform layer was extracted with water (20 ml.). The aqueous layer was washed twice with chloroform (5 ml.) and concentrated under reduced pressure to recover the same object compound (0.43 g.).

Provenance & Evidence