HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-[(2,4,6-Trimethylphenyl)methylene]propanedinitrile → HCID 67214165, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-[(2,4,6-Trimethylphenyl)methylene]propanedinitrile | HCID 593057 | — |
| Reactant | HCID 33777858 | HCID 33777858 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 67214165 | HCID 67214165 | — |
Reaction Steps
A solution of 284 mg (2.01 mmol) of 4,6-dihydro-1H-thieno[3,4-c]pyrazol-3-amine (Intermediate 21) and 395 mg (2.01 mmol) of (mesitylmethylene)malononitrile (Intermediate 3) in 5 mL of anhydrous pyridine was stirred at reflux under air overnight (protected from moisture with a calcium sulfate drying tube) and then cooled and concentrated in vacuo. The residue was stirred with 20 mL of methanol and filtered to remove some insoluble material, which was washed with an additional 5 mL of methanol. The combined filtrate and washings were concentrated. Purification of the residue by flash chromatography on silica gel (gradient elution with 5-15% ethyl acetate in hexane) afforded the title compound as a solid. LC-MS 336 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07956061B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-a51459df63c345b89d2f493e1d48b7a3 |
| Source note | uspto-grants-2011_06 |