Bromotrimethylsilane → HCID 20337186, compound

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.).

1. concentrationSubsequently, the reaction mixture was concentrated under reduced pressure
2. customto give a residue
3. stirringAfter the mixture was stirred for an hour at ambient temperature
4. washthe mixture was washed three times with chloroform (10 ml.)
5. concentrationconcentrated under reduced pressure

ORD record

ord-61f8f6583ca14d938caffd07a0867a3a

Source dataset

uspto-grants-1980_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04206156