Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 178525132 | HCID 178525132 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 178419939 | HCID 178419939 | — |
Reaction Steps
To a solution of A5′ (2.5 g, 3.5 mmol) in o-xylene (25 mL) in a sealed tube was added ammonium acetate (4.1 g, 53 mmol). The mixture was sealed and heated at 140° C. for 3 h and then cooled to rt. The volatile component was removed in vacuo, and the residue was partitioned between H2O and CH2Cl2, and the organic phase was dried, filtered and concentrated in vacuo. The resulting crude material was purified by silica gel column chromatography (CH2Cl2/MeOH=9/1 (v/v)) to provide A6′ as a yellow solid (250 mg, 10% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09120779B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-ec38b1a99d4f487593bc0951b20dca57 |
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| Source note | uspto-grants-2015_09 |
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