Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | 1,4-dihydro-3H-2-benzopyran-3-one | HCID 78092 | — |
| Product | HCID 66961648 | HCID 66961648 | — |
Reaction Steps
An ethanol solution of hydrogen bromide (25%, 10 ml) was added to 1,4-dihydro-3H-isochromene-3-one (500 mg) and stirred at 70° C. overnight. After removing the solvent, the residue was roughly purified with a silica gel chromatography (hexane-ethyl acetate) to obtain a crude material of [2-(bromomethyl)phenyl]ethyl acetate. Methyl 3-(4-aminophenyl)-2-[(2,6-dichlorobenzoyl)amino]propionate (520 mg), triethylamine (490 μl) and DMF (5 ml) were added to the crude material and stirred at 125° C. for six hours. After removing the solvent, the residue was purified with a silica gel chromatography (hexane-ethyl acetate) to obtain methyl 2-[(2,6-dichlorobenzoyl)amino]-3-(4-{[2-(2-ethoxy-2-oxoethyl)benzyl]amino}phenyl)propionate (510 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07884204B2 |
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| Source dataset | uspto-grants-2011_02 |
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| ORD ID | ord-b6c655aaf6b749639796c2956505de61 |
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| Source note | uspto-grants-2011_02 |
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