HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 86620138, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 86620139 | HCID 86620139 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 86620138 | HCID 86620138 | 95.4% |
Reaction Steps
Methanesulfonic acid (0.30 mL, 4.63 mmol) was added to a solution of tert-butyl [(6S,9R)-6-(2,3-difluorophenyl)-3-(1-methoxy-1-methylethyl)-6,7,8,9-tetrahydro-5H-imidazo[1,2-a]azepin-9-yl]carbamate (50 mg, 0.115 mmol) and sodium azide (170 mg, 2.62 mmol) in chloroform (10 mL). After 1 h, additional methanesulfonic acid (0.95 mL, 14.65 mmol) was added. After 16 h, the reaction mixture was concentrated. Purification by reverse phase HPLC (100% water→100% acetonitrile with 0.1% trifluoroacetic acid) gave the title compound (38 mg). MS 347.1 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08039460B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-c25c915f04494188bfe5f939636f933d |
| Source note | uspto-grants-2011_10 |