Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 118676857 | HCID 118676857 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 118676845 | HCID 118676845 | — |
Reaction Steps
Sodium azide (0.31 g, 4.79 mmol) was added to a solution of 68a) (0.75 g, 1.37 mmol) in DMF (8.65 mL) and the resulting mixture was stirred at 60° C. for 2 h. After cooling to ambient temperature, the reaction mixture was poured onto water and extracted with dichloromethane (3×30 mL). The organic phase was dried over sodium sulfate and concentrated. The remnant was purified by flash column chromatography [silica; 2.5% methanol in dichloromethane]. White solid. Yield: 0.4 g (59% of theory). HPLC-MS (method 4): Rt=3.04 min; m/z [M+H]+=490.2
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09315490B2 |
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| Source dataset | uspto-grants-2016_04 |
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| ORD ID | ord-7bfa09defc414c1da2431bd0ce59ba34 |
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| Source note | uspto-grants-2016_04 |
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