HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 10535422, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methyl 3-aminocrotonate | HCID 643918 | — |
| Reactant | HCID 57361639 | HCID 57361639 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10535422 | HCID 10535422 | 15.6% |
Reaction Steps
4,5-Dichloro-[1,2,3]-dithiazol-1-ylium chloride (prepared according to Chem. Ber. (1985) 118, 1632) (8.34 g, 40 mmol) was dissolved in dichloromethane (30 ml) and methyl-3-aminocrotonate (4.6 g, 40 mmol) was added dropwise at room temperature. After stirring the solution for 1 hour at room temperature pyridine (6.47 ml, 80 mmol) was added slowly. The mixture was concentrated and purified by chromatography on silica gel (eluent: ethyl acetate/hexane) to give the product as an orange solid (1.14 g, 15.6% yield). 1H-NMR (400 MHz, CDCl3): 2.88 (3H, s, Me), 4.0 (3H, s, Me).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680290B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-8c1b3e34fedd4eacb9861520d0705283 |
| Source note | uspto-grants-2014_03 |