HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium bicarbonate → Methyl (methylethoxycarbonyloxy)ethyl (2E)but-2-ene-1,4-dioate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium bicarbonate | HCID 2734983 | — |
| Reactant | Monomethyl Fumarate | HCID 5369209 | — |
| Reactant | 2-Chloroethyl propan-2-yl carbonate | HCID 19765119 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | Methyl (methylethoxycarbonyloxy)ethyl (2E)but-2-ene-1,4-dioate | HCID 73295994 | 91% |
Reaction Steps
Following general procedure A, methyl hydrogen fumarate (0.39 g, 3.0 mmol) in NMP (8 mL) was reacted with CsHCO3 (0.69 g, 3.6 mmol) and methylethyl (chloroethoxy)formate (0.70 g, 4.2 mmol) to afford 0.71 g (91% yield) of the title compound (40) after isolation and purification. 1H NMR (CDCl3, 400 MHz): δ 6.89 (d, J=15.6 Hz, 1H), 6.84 (q, J=5.2 Hz, 1H, superimposed), 6.82 (d, J=15.6 Hz, 1H, superimposed), 4.90 (heptet, J=6.2 Hz, 3H), 3.81 (s, 3H), 1.57 (d, J=5.2 Hz, 3H), 1.32 (d, J=6.2 Hz, 3H), 1.31 (d, J=6.2 Hz, 3H). MS (ESI): m/z 261.02 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785443B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-4e643b9bf3dd497db1ecad354a97de12 |
| Source note | uspto-grants-2014_07 |