Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester | HCID 17453 | — |
| Reactant | HCID 67279997 | HCID 67279997 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86641343 | HCID 86641343 | 33.3% |
Reaction Steps
A mixture composed of di-tert-butyl {2-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-8-oxo-2,7,8,9-tetrahydro-6-thia-1,2,3,5-tetraazabenzo[cd]azulen-4-yl}imidodicarbonate of Example 40 (752 mg), methyl triphenylphosphanylideneacetate (617 mg) and toluene (14 ml) was heated with stirring at 60° C. for 10 hours. Ethyl acetate was added to the reaction mixture, followed by washing with water. Then, the organic layer was dried over sodium sulfate and filtered, and then the filtrate was concentrated under reduced pressure. The concentrated residue was purified by silica gel column chromatography (ethyl acetate-chloroform) to obtain the title compound (275 mg, 33%) as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08158638B2 |
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| Source dataset | uspto-grants-2012_04 |
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| ORD ID | ord-6a93103d71b04610b038d906a3977594 |
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| Source note | uspto-grants-2012_04 |
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