Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | HCID 178478337 | HCID 178478337 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178514340 | HCID 178514340 | — |
Reaction Steps
To a stirred solution of 9-2 (5 g, 8.9 mMol) in anhydrous 1,4-dioxane (20 mL) was added hydrazine (5.9 mL, 188.1 mMol). The solution was heated to 100° C. in a microwave reactor for 5 minutes. The solvent was removed in vacuo and was dried azeotropically with toluene three times. The crude solid was triturated with a saturated NaHCO3 solution for 20 minutes. The suspension was filtered and washed with copious amounts of water. The solid was dried azeotropically with toluene three times to yield 9-3 as a tan solid. LC/MS (M+1) calculated: 554.6; observed: 554.2
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08008317B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-8f08756f0333433ca60b4c3330ce2090 |
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| Source note | uspto-grants-2011_08 |
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