Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 58959113 | HCID 58959113 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 58959127 | HCID 58959127 | — |
Reaction Steps
A solution of compound 5.6 (28.8 mg, 0.057 mmol) in MeOH (3 mL) was transferred to a steel bomb, cooled to −50 to −60° C., and treated with a saturated solution of ammonia in MeOH (10 mL). The reactor was sealed and heated at 118° C. overnight. The reaction vessel was cooled (0-5° C.), opened carefully and the reaction mixture was evaporated to dryness. The crude product was dissolved in MeOH, adsorbed onto silica gel and purified by flash column chromatography on silica gel using pure CH2Cl2 to 4% MeOH in CH2Cl2 as eluents to give the desired compound 5.7 (20.7 mg) as an off white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07268119B2 |
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| Source dataset | uspto-grants-2007_09 |
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| ORD ID | ord-86b4c128ddb3478b8d12a93997e78cc7 |
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| Source note | uspto-grants-2007_09 |
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