HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 86698012, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Fluoro-1-nitro-2-(propan-2-yloxy)benzene | HCID 10631832 | — |
| Reactant | 1-Methyl-1,7-diazaspiro[4.4]nonane | HCID 52988115 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86698012 | HCID 86698012 | 7% |
Reaction Steps
A mixture of 1.42 g of 4-fluoro-1-nitro-2-(propan-2-yloxy)benzene, 1.0 g of 1-methyl-1,7-diazaspiro[4,4]nonane and 1.48 g of potassium carbonate in 10 ml of DMSO is stirred at ambient temperature overnight. The mixture is diluted with 160 ml of water and extracted three times with 100 ml of ethyl acetate. The organic phases are dried over magnesium sulfate and concentrated under vacuum. The yellow oily residue is purified on silica, with an elution gradient with dichloromethane/methanol (100/0 then 90/10), so as to obtain 160 mg of 1-methyl-7-[4-nitro-3-(propan-2-yloxy)phenyl]-1,7-diazaspiro[4.4]nonane in the form of an orangey-coloured oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115140B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-8d2076da8abf4742b6dc55e27a221b8e |
| Source note | uspto-grants-2015_08 |