HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 53248105, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Maleic Anhydride | HCID 7923 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 53248162 | HCID 53248162 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 53248105 | HCID 53248105 | 83% |
Reaction Steps
4-(Tert-butoxycarbonylamino)-3-sulfobutanoic acid (321 mg, 1.13 mmol) was stirred in the mixture of HCl (conc)/Dioxane (1:4, 15 ml) for 30 min, evaporated and coevaporated with EtOH/Toluene (1:1, 4×20 ml) to dryness. To the dryness material was added maleic anhydride (121 mg, 1.23 mmol) and DMA (20 ml) and the mixture was stirred overnight, evaporated and run through C-18 column eluted with water and crystallized with EtOH/Hexane to afford 263 mg (83%) of the title compound. ESI MS 279.8 (M−H). The NMR data are the same through the route with 4-azido-3-sulfobutanoic acid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236319B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-dd47d1b2c9c34da483474007ec8960c1 |
| Source note | uspto-grants-2012_08 |