HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Hydroxide → HCID 178492295, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | 5-[(3,4-Dimethoxy-phenylamino)-methylsulfanyl-methylene]-2,2-dimethyl-[1,3]dioxane-4,6-dione | HCID 57810094 | — |
| Catalyst | Mercuric Chloride | HCID 24085 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178492295 | HCID 178492295 | 97% |
Reaction Steps
A mixture of 5-[(3,4-dimethoxy-phenylamino)-methylsulfanyl-methylene]-2,2-dimethyl-[1,3]dioxane-4,6-dione (1.0 g, 2.8 mmol), 30% ammonium hydroxide (8.5 mL), HgCl2 (0.75 g, 2.8 mmol) in THF (5 mL) was stirred at room temperature for 30 minutes. The mixture was extracted with DCM and water (3×) and dried with Na2SO4. Concentration in vacuo afforded 5-[amino-(3,4-dimethoxy-phenylamino)-methylene]-2,2-dimethyl-[1,3]dioxane-4,6-dione as a white solid (0.90 g, 97% yield) and this compound was used without further purification. LCMS: m/z 321 (M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09174947B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-2c364d3c41254de2a7328da92836da17 |
| Source note | uspto-grants-2015_11 |