HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 66808394, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-Bromobenzene-1,2-diamine | HCID 323593 | — |
| Reactant | HCID 22120960 | HCID 22120960 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66808394 | HCID 66808394 | 51.6% |
Reaction Steps
A solution of 4-bromo-1,2-benzenediamine (214 mg, 1.145 mmol) in N,N-dimethylformamide (12 mL) containing water (0.4 mL) was treated with the product of Example 147A (400 mg, 1.145 mmol) and OXONE (458 mg, 0.7443 mmol), and the reaction stirred at room temperature for 30 minutes. Water (40 mL) was then added and the reaction stirred for 10 minutes. The mixture was vacuum filtered and the solid washed with water, then dried under vacuum. Purification by silica gel chromatography using a gradient of 3% to 4% ethyl acetate/methylene chloride as eluent provided the title compound as a yellow solid (305 mg, 51%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07915411B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-c8ac34ff127c46eeabb538b2403d852f |
| Source note | uspto-grants-2011_03 |