HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Chlorite → HCID 89662736, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Chlorite | HCID 23668197 | — |
| Reactant | Monosodium phosphate | HCID 23672064 | — |
| Reactant | HCID 131736544 | HCID 131736544 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 89662736 | HCID 89662736 | 84% |
Reaction Steps
A solution of sodium chlorite (214 mg; 2.36 mmol; 5.5 eq.) and sodium dihydrogenphosphate (186 mg; 1.55 mmol; 3.6 eq.) in water (2 mL) was added dropwise to a mixture of 4-(2-formyl-phenyl)-7-trifluoromethyl-[1,4]diazepane-1-carboxylic acid tert-butyl ester (160 mg; 0.43 mmol; 1 eq.) in 1,4-dioxane (2 mL). The reaction mixture was stirred at room temperature for 1 hour and the 1,4-dioxane concentrated in vacuo. The aqueous solution was diluted with water, the pH made acidic with 0.1M HCl and extracted with EA (2×). The combined organic layer was washed with brine, dried over magnesium sulfate and concentrated in vacuo to afford the title compound (140 mg, 84%) as a yellow solid. UPLC/MS: (MS+) 389.2 ([M+H]+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09403835B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-5058ae34a1174149bb417d5962803edb |
| Source note | uspto-grants-2016_08 |