HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 44155564, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 66799768 | HCID 66799768 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 44155564 | HCID 44155564 | 87% |
Reaction Steps
To a solution of [3-(9-fluoro-4H,6H-2,3,5,10b tetraaza-benzo[e]-azulen-5-yl)-3-oxo-1-(2,4,5-trifluoro-benzyl)-propyl]-carbamic acid-tert-butyl ester, (2.04 g, 3.93 mmol); in dry DCM (12 mL) was added trifluoroacetic acid (11.79 mL, 3 mL/mmol) at 0° C. The reaction mixture was stirred at r.t. for 2 h under argon. After completion of the reaction as confirmed by TLC, methanol (2×5 mL) was added and the reaction mixture was evaporated under vacuo to remove excess of solvent and trifluoroacetic acid. The remaining solvents were removed under vacuo to obtain trifluoroacetic acid salt of (R)-3-amino-1-(9-fluoro-4H,6H-2,3,5,10b-tetraaza-benzo[e]azulen-5-yl)-4-(2,4,5-trifluoro-phenyl)-butan-1-one as a white solid (1.82 g, 3.42 mmol, 87%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08455479B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-c5580a6dfcc44027b42eb98fd1a1baa4 |
| Source note | uspto-grants-2013_06 |