HuagongsheHuagongshe Chemistry Print Report · For research reference only
Fumaric Acid → HCID 86639360, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Fumaric Acid | HCID 444972 | — |
| Reactant | HCID 520648 | HCID 520648 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 86639360 | HCID 86639360 | 12.1% |
Reaction Steps
Following general procedure A, chloroethyl 2-methylpropanoate (0.24 g, 1.58 mmol) was reacted overnight with the pre-formed bis-dicyclohexylamine salt (DCHA) of fumaric acid (FA) (0.50 g, 1.26 mmol) in N-methylpyrrolidinone (NMP) at ca 100° C. The crude material was purified by mass-guided preparative HPLC to afford (0.035 g, 12% yield) of the title compound (49) as a white, waxy, semi-solid. 1H NMR (CD3CN, 400 MHz): δ 6.89-6.83 (q, J=5.6 Hz, 1H), 6.82-6.81 (d, J=16.0 Hz, 1H), 6.73-6.69 (d, J=16.0 Hz, 1H), 2.58-2.49 (heptet, J=6.8 Hz, 1H), 1.49-1.47 (d, J=5.6 Hz, 3H), 1.12 (d, J=7.2 Hz, 3H), 1.09 (d, J=6.8 Hz, 6H); MS (ESI): m/z=239.01 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785443B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-ea3a354ca714413ca11988de133bed16 |
| Source note | uspto-grants-2014_07 |