Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Acetic-formic anhydride | HCID 75269 | — |
| Reactant | HCID 23368525 | HCID 23368525 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23368378 | HCID 23368378 | — |
Reaction Steps
To a solution of 1 g of 3-(2-aminopentyloxy)-5-chloro-1,2-benzoisoxazole in 10 ml of methylene chloride is added 0.42 g of acetic formic anhydride with ice-cooling, and they are subjected to reaction at room temperature for one hour. The solvent is removed by distillation under reduced pressure, and water and ethyl acetate are added to the residue obtained, and the pH is adjusted to 8 with a 20% (w/w) aqueous sodium hydroxide solution. After shaking, the organic layer is separated. The separated organic layer is washed with a saturated saline solution and dried over anhydrous magnesium sulfate, after which the solvent is removed by distillation under reduced pressure, to obtain 1.1 g of colorless, crystalline 5-chloro-3-(2-formylaminopentyloxy)-1,2-benzoisoxazole having a melting point of 107.2°-108.3° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05578627 |
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| Source dataset | uspto-grants-1996_11 |
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| ORD ID | ord-a565592b530842beba6628e373c90500 |
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| Source note | uspto-grants-1996_11 |
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