HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 9958543, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Dimedone | HCID 31358 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 12052587 | HCID 12052587 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 9958543 | HCID 9958543 | 87.1% |
Reaction Steps
Compound 6 (490 mg, 0.86 mmole) was dissolved in DMF (9 mL). 5,5-Dimethyl-1,3-cyclohexanedione (181 mg, 1.29 mmole), N,N-diisopropylethylamine (0.225 mL, 1.29 mmole) and (tetrakistriphenylphoshine)palladium (50 mg, 0.043 mmole) were then added and the solution stirred for 2 hours. Then aqueous ammonium chloride was added and the solution was extracted repeatedly with dichloromethane. The combined organics were dried over sodium sulfate, filtered and the filtrate was evaporated . The crude isolate was then purified by silica gel chromatography to give the title compound (395 mg, 87%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06525083B2 |
| Source dataset | uspto-grants-2003_02 |
| ORD ID | ord-a4f1bf715c02432796828b3948f3d213 |
| Source note | uspto-grants-2003_02 |