HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 71237041, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 71237441 | HCID 71237441 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 71237041 | HCID 71237041 | 102% |
Reaction Steps
Add trifluoroacetic acid (30 mL, 396.76 mmol) over 5 minutes to a 0° C. solution of tert-butyl N-[(1S)-2-[[5-[2-(tert-butyl(dimethyl)silyl)oxyethyl]-6-oxo-7H-pyrido[2,3-d][3]benzazepin-7-yl]amino]-1-methyl-2-oxo-ethyl]carbamate (5.56 g, 10.0 mmol) and dichloromethane (30 mL) and allow to warm and stir at ambient temperature for 5 hours. Purify the residue by flash chromatography via SCX® columns (Isolute SCX-2×6) eluting with methanol followed by ethyl acetate: methanol (2N ammonia) (1:1) to obtain the title compound as a white solid (3.48 g, 10.2 mmol) in quantitative yield. MS (m/z): 341 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08569286B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-50f29f9d58d14d149c225e0481116191 |
| Source note | uspto-grants-2013_10 |