HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfamic Acid → HCID 89725527, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfamic Acid | HCID 5987 | — |
| Reactant | HCID 13343417 | HCID 13343417 | — |
| Reactant | Sodium Chlorite | HCID 23668197 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 89725527 | HCID 89725527 | — |
Reaction Steps
Ethyl 5-formylbenzofuran-2-carboxylate (3.8 g, 17.4 mmol) was dissolved in a mixture of THF (80 mL) and t-BuOH (20 mL). A solution of sulfamic acid (4.0 g, 41.2 mmol) and sodium chlorite (3.4 g, 37.6 mmol) in water (70 mL) was added dropwise at RT. After 3 h an additional portion of sulfamic acid (1.2 g) and sodium chlorite (1.4 g) in water was added in one portion. The reaction mixture was stirred overnight at RT, then extracted twice with EtOAc, dried over sodium sulfate and concentrated under vacuum to give the crude product, 4.87 g which was suitable for use without purification. 1H NMR (DMSO-d6) 8.42 (m, 1H), 8.07 (m, 1H), 7.49-7.81 (m, 2H), 4.37 (q, 2H, OCH2), 1.34 (t, 3H, OCH2CH3); m/z 234.94 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09409884B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-6f7a6a71e97e461a8b0b11c3b466e66f |
| Source note | uspto-grants-2016_08 |