HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 86607458, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | HCID 86607459 | HCID 86607459 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86607458 | HCID 86607458 | — |
Reaction Steps
A mixture of 0.359 g (1.4 mmol) of N-(cyclohexyl)diethylphosphonoformamide, 0.276 g (0.7 mmol) of Lawesson Reagent in 10 ml toluene was refluxed for 5.5 hours. The resulting mixture was subjected to VLC (vacuum liquid chromatography) using gradient eluants (from 5% ethyl acetate in petroleum ether to ethyl acetate/petroleum ether (40:60) to give N-cyclohexyl diethylphosphonothioformamide as a yellow solid, 0.327 g (85.8%, isolated yield). NMR (CDCl3): 31P −1.66. 1H: 1.18-2.01 (m, 16H), 4.17 (m, 4H), 4.34 (m, 1H), 8.89 (br. s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07468359B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-cbb6161f3879424fafc91a134308db83 |
| Source note | uspto-grants-2008_12 |