Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 67344504 | HCID 67344504 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 57668008 | HCID 57668008 | — |
Reaction Steps
To dichloromethane 5.0 mL solution of 2-methyl-5-phenoxyaniline hydrochloride 0.50 g were added pyridine 0.34 mL and acetic anhydride 0.24 mL under ice cooling, and it was stirred at room temperature for 6 hours and 30 minutes. The solvent was removed under reduced pressure,1.0 mol/L hydrochloric acid and ethyl acetate were added to the obtained residue. The organic layer was separated and collected,dried over anhydrous magnesium sulfate after sequential washing with saturated sodium hydrogen carbonate aqueous solution and saturated sodium chloride aqueous solution, and the solvent was removed under reduced pressure. The obtained residue was refined by silica gel column chromatography [Fuji SILYSIA Chemical Ltd., PSQ100B(spherical type), eluent; hexane:ethyl acetate=2:1] to give N-(2-methyl-5-phenoxyphenyl)acetamide 0.44 g of white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08327467B2 |
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| Source dataset | uspto-grants-2012_12 |
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| ORD ID | ord-df8c586996334f85ac4501e6fb63e7a4 |
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| Source note | uspto-grants-2012_12 |
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