HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl vinylphosphonate → HCID 10903865, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl vinylphosphonate | HCID 69629 | — |
| Reactant | tert-Butyl (3-aminopropyl)carbamate | HCID 2735700 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 10903865 | HCID 10903865 | 81.3% |
Reaction Steps
To a solution of 3-(t-butyloxycarbonylamino) propanamine (77 g, 0.44 mole) in methanol (500 mL) was added diethyl vinylphosphonate 97% (75 g, 0.44 mole; Aldrich 11, 613-0) under nitrogen and kept in a water bath at ~20° C. for 48 hr. The reaction mixture was concentrated in vacua and the residue (~160 g) was put on a pad of "Florisil" (3"×6") and eluted with methylene chloride/hexane 1:1, methylene chloride and finally 10% methanol/methylene chloride to give the title compound as a colorless oil (121 g, 80%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06011168 |
| Source dataset | uspto-grants-2000_01 |
| ORD ID | ord-636a50876eba4c63b43dc697d15d5c6d |
| Source note | uspto-grants-2000_01 |