HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 72713171, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Sodium bicarbonate water | HCID 86585896 | — |
| Reactant | HCID 131736367 | HCID 131736367 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 72713171 | HCID 72713171 | 99.4% |
Reaction Steps
TFA (37.0 g, 25 mL, 324 mmol, Eq: 55.9) was added dropwise over 2 h to a solution of tert-butyl (S)-1-((S)-5-((2-cyano-1-(2-cyanophenyl)-1H-indol-3-yl)methyl)-4-oxo-2′,3′,4,5,5′,6′-hexahydro-3H-spiro[benzo[b][1,4]oxazepine-2,4′-pyran]-3-ylamino)-1-oxopropan-2-yl(methyl)carbamate (4 g, 5.81 mmol) in DCM (50 mL) at 0° C. After 30 min. the mixture was added to sat. NaHCO3/H2O 1:1, the organic phase was separated, dried over Na2SO4, filtered and concentration to give the title compound (3.4 g, 97%) as a light yellow solid. MS m/z 589 (MH+)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09394263B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-162aff8d198842f38f0171112ff93565 |
| Source note | uspto-grants-2016_07 |