Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 178422859 | HCID 178422859 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 11789279 | HCID 11789279 | — |
Reaction Steps
9.70 g of 5-hydroxy-3-methyl-4-(3-methylisooxazol-5-yl)isoxazole was added to 18 ml of acetic acid and 30 ml of methanol, and was heated to 60° C. to dissolve. To the resulting solution was added 3.20 g of electrolytic iron powder to stir for an hour at 60° C. 20 ml of 3N hydrochloric acid was further added to the reaction solution to stir for 20 minutes at 60° C. The reaction mixture was cooled to room temperature and water was added. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated salt water, dried over anhydrous magnesium sulfate and concentrated to give 6.00 g of the title compound as a reddish brown liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06359143B1 |
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| Source dataset | uspto-grants-2002_03 |
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| ORD ID | ord-39d0e7c5ad944146a38f0d09853d1265 |
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| Source note | uspto-grants-2002_03 |
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