HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 71539919, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 86680060 | HCID 86680060 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 71539919 | HCID 71539919 | 73.2% |
Reaction Steps
A solution of tert-butyl (R)-4-(4-(5-(tert-butoxycarbonylamino)-2-(2,6-difluorophenyl)thiazole-4-carboxamido)-1-methyl-1H-pyrazol-5-yl)-2-methylpiperazine-1-carboxylate (80 mg, 0.126 mmol) in TFA (1 mL) and DCM (4 mL) was stirred at ambient temperature for 3 hours. The pH of the mixture was adjusted to about 8˜9 by addition of ammonia and concentrated under reduced pressure to give a residue. The residue was purified by preparative HPLC to afford 102 (40 mg, 73%). 1H NMR (500 MHz, CDCl3) δ (ppm): 8.48 (s, 1H), 8.33 (s, 1H), 7.69 (s, 1H), 7.30-7.36 (m, 1H), 7.03-7.07 (m, 2H), 6.14-6.17 (m, 2H), 3.78 (s, 3H), 3.53-3.48 (m, 1H), 2.90-3.34 (m, 6H), 1.32 (d, J=6.5 Hz, 3H); MS (ESI) m/z=434 (M+1+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08614206B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-32eafacc0bf74b51b6e3eb9611df3463 |
| Source note | uspto-grants-2013_12 |