HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 178481674, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | Methylthiourea | HCID 2723704 | — |
| Reactant | Ethyl 3-(4-pyridyl)-3-oxopropionate | HCID 2735202 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178481674 | HCID 178481674 | 72.1% |
Reaction Steps
A solution of ethyl 3-oxo-3-(4-pyridyl)propionate (29.0 g, 150 mmol), N-methyl thiourea (40.6 g, 450 mmol) and 1,8-diazabicyclo[5,4,0]-7-undecene (22.4 ml, 150 mmol) was refluxed for 4 hours and the solution of methanesulfonic acid (14.4 g, 150 mmol) in water (50 ml) was added after cooling by ice-water. The precipitate was washed with water, filtered and dried to give the title compound (23.7 g, 72%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07504411B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-943eca4e9b374abaa48b3e4858d24a84 |
| Source note | uspto-grants-2009_03 |