HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 59134447, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 68540889 | HCID 68540889 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59134447 | HCID 59134447 | — |
Reaction Steps
Bubble gaseous hydrochloric acid through a solution of 4-(6-methyl-5-{3-[5-(1-methyl-cyclopropyl)-2-p-tolyl-2H-pyrazol-3-yl]-ureido}-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (assume 2.74 mmol) in 1:1 ethyl acetate:dichloromethane (200 mL) for 3 min to ensure saturation. Allow the mixture to stand for 30 min then concentrate under reduced pressure to a white solid. Dissolve the solid in MeOH and load onto a 20 g Varian SCX column, rinsing with additional MeOH. Elute the free base with 1:1 2 M ammonia in MeOH:dichloromethane. Concentrate the solution under reduced pressure to give a white solid (1.21 g, 99% over 2 steps). LCMS(ES+): m/z=446 [M+H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652015B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-adc5ea69b8084753a856298e5177121d |
| Source note | uspto-grants-2010_01 |