Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | HCID 86620133 | HCID 86620133 | — |
| Product | HCID 59722543 | HCID 59722543 | — |
Reaction Steps
Methanesulfonic acid (78 μL, 1.19 mmol) was added to a solution of tert-butyl [(6S,9R)-6-(2,6-difluorophenyl)-3-(1-methoxy-1-methylethyl)-6,7,8,9-tetrahydro-5H-imidazo[1,2-a]azepin-9-yl]carbamate (104 mg, 0.24 mmol) in ethylene glycol (4 mL) and the mixture heated to 60° C. After 18 h, the reaction mixture was concentrated. Saturated aqueous sodium bicarbonate was added and the mixture was extracted with dichloromethane (3×), and the combined organic extracts were washed with saturated brine, dried over sodium sulfate, filtered and concentrated. MS 366.1 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08039460B2 |
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| Source dataset | uspto-grants-2011_10 |
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| ORD ID | ord-6de7ac219a2040098175b3420931e55e |
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| Source note | uspto-grants-2011_10 |
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