Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 2111998 | HCID 2111998 | — |
| Reactant | Magnesium Chloride | HCID 5360315 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 178441029 | HCID 178441029 | — |
Reaction Steps
The product from Example 4A (300 mg, 1.08 mmol) in N,N-dimethylacetamide (10 mL) was treated with NaN3 (0.7 g, 10.8 mmol) and MgCl2 (1.03 g, 10.8 mmol). The mixture was heated at 150° C. for 16 hours, allowed to cool to room temperature, and poured into H2O (50 mL). The mixture was filtered and the filter cake air-dried to provide the title compound as a solid. 1H NMR (300 MHz, DMSO-d6) δ 10.14 (s, 1H), 8.10 (d, J=8.4 Hz, 2H), 7.97 (d, J=8.4 Hz, 2H), 7.71 (d, J=8.5 Hz, 2H), 7.36 (d, J=8.4 Hz, 2H), 1.29 (s, 9H); MS (ESI+) m/z 322 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07595332B2 |
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| Source dataset | uspto-grants-2009_09 |
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| ORD ID | ord-a6b9ce3100184e3cbc5cf499209c2922 |
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| Source note | uspto-grants-2009_09 |
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