HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Isothiocyanato-4-methylthiophene → HCID 22139854, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Isothiocyanato-4-methylthiophene | HCID 22139827 | — |
| Reactant | HCID 22139851 | HCID 22139851 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22139854 | HCID 22139854 | — |
Reaction Steps
A solution of 3-isothiocyanato-4-methylthiophene (296.2 mg, see example 1a) in absolute tetrahydrofuran (10 ml) was added dropwise to a solution of 1,4-dioxaspiro[4.5]dec-6-ylamine (300 mg) in absolute tetrahydrofuran (10 ml), the mixture was stirred at room temperature for 2 hours and the solvent was then removed under reduced pressure. The residue was purified by preparative chromatography and the product-containing fractions were combined, freed from acetonitrile, made basic and extracted three times with ethyl acetate. The organic phases were combined, dried (MgSO4) and filtered. This gave 428 mg of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07317033B2 |
| Source dataset | uspto-grants-2008_01 |
| ORD ID | ord-7d1a3db3229f465ab7e594b22fe34b82 |
| Source note | uspto-grants-2008_01 |