Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 68863478 | HCID 68863478 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 68862592 | HCID 68862592 | — |
Reaction Steps
Acetyl chloride (0.17 ml) was added to a mixture of the compound of Example 42 (0.83 g), ethyldiisopropylamine (1.05 ml) and dioxane (10 ml) at 0° C., allowed to be warmed to 25° C. and stirred for 9 days. The solvent was evaporated under reduced pressure. The residue was diluted with ethyl acetate and washed with 1 M hydrochloric acid and saturated brine. The organic layer was dried over MgSO4, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform) and recrystallized from ethyl acetate/hexane, thereby giving 0.25 g of the desired compound. Melting point: 233-235° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07514452B2 |
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| Source dataset | uspto-grants-2009_04 |
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| ORD ID | ord-cb569979601b464c9b3da2caef1fb051 |
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| Source note | uspto-grants-2009_04 |
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