HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 20695532, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Silane, tris(1-methylethyl)- | HCID 138754 | — |
| Reactant | HCID 86585964 | HCID 86585964 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 20695532 | HCID 20695532 | — |
Reaction Steps
A solution of ethyl 2-{{2-chloro-5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-4-fluorophenyl}imino}-4-oxo-5-{[(trityloxy)carbamoyl]-methyl}-3-thiazolidineacetate (entire sample from Example 23) and triisopropylsilane (1 mL) in trifluoroacetic acid (19 mL) is stirred at room temperature for 4 hours, cooled with an ice-water bath, and filtered. The resultant filtrate is concentrated in vacuo and chased three times with toluene to obtain a solid. Column chromatography of the solid using silica gel and a 7.5% methanol in methylene chloride solution gives the title product as a yellow solid which is identified by 1H NMR spectral analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06303783B1 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-0413268f571d4b69a0a302f038bb4f70 |
| Source note | uspto-grants-2001_10 |