Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 18399304 | HCID 18399304 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18399332 | HCID 18399332 | — |
Reaction Steps
A solution of the compound obtained in Example 68 (200 mg) and triethylamine (145 μd) in tetrahydrofuran (15 ml) is cooled to −20° C., and thereto is added a solution of acetyl chloride (61 mg) in tetrahydrofuran (5 ml). The reaction mixture is stirred at the same temperature for one hour, and warmed to room temperature. To the reaction mixture are added acetyl chloride (122 mg) and triethylamine (290 μl), and the mixture is stirred at room temperature overnight. To the reaction mixture are added ethyl acetate and water, and the ethyl acetate layer is separated, washed, dried, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (solvent; hexane:ethyl acetate=2:1) to give 2-diacetylamino-3-methoxycarbonyl-4-(3,4,5-trimethoxyphenyl)-1(2H)-isoquinolinone (75 mg) as listed in Table 6.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06486155B1 |
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| Source dataset | uspto-grants-2002_11 |
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| ORD ID | ord-23be52011f5140b494c46d4109e78d7f |
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| Source note | uspto-grants-2002_11 |
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