HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → HCID 22466474, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | 6-Chloro-2-propoxy-3-propylthieno[2,3-d]pyrimidin-4(3H)-one | HCID 22466475 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 22466474 | HCID 22466474 | — |
Reaction Steps
In a sulfonation flask, a mixture of 1.15 g 6-chloro-2-propoxy-3-propyl-4-oxo-thieno[2,3-d]pyrimidine, 0.97g Lawesson reagent and 50 ml of dioxane is heated at reflux temperature for 3.5 hours. After removal of the solvent in the water jet vacuum, the residue is taken up in ethylacetate and the organic phase is washed twice with water. The organic phase is dried over sodium sulfate and the solvent removed in the water jet vacuum. The crude material is purified twice by column chromatography over silica gel (eluant: tert. butylmethylether/hexane 1:9). Yield: 0.3 g pure 6-chloro-2-propoxy-3-propyl-4thioxo-thieno[2,3-d]pyrimidine in the form of a yellow powder; m.p. 81-83° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06384040B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-03cab8804c8f4ad680718685cd8a43bb |
| Source note | uspto-grants-2002_05 |