Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trichloroacetyl isocyanate | HCID 76400 | — |
| Reactant | HCID 23368483 | HCID 23368483 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23368409 | HCID 23368409 | — |
Reaction Steps
To a solution of 0.58 g of 3-(2-tert-butoxycarbonylamino-3-hydroxypropoxy)-5-dimethylamino-1,2-benzoisoxazole in 12 ml of methylene chloride is added 0.26 g of trichloroacetyl isocyanate at -35° to -30° C., and the temperature is elevated to 0° C., after which they are subjected to reaction at the same temperature for one hour. To the reaction mixture is added 10 ml of water, and they are subjected to reaction at 20°-25° C. for one hour, after which the organic layer is separated. The separated organic layer is dried over anhydrous magnesium sulfate and thereafter the solvent is removed by distillation under reduced pressure, to obtain 0.94 g of brown, oily 3-(3-carbamoyloxy-2-tert-butoxycarbonylaminopropoxy)-5-dimethylamino-1,2-benzoisoxazole.
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-a347d9399aba4ac3bbb597da2ab5290b |
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| Source note | uspto-grants-1996_11 |
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