HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 10279422, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 69421103 | HCID 69421103 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 10279422 | HCID 10279422 | 19.1% |
Reaction Steps
A solution of [1-{4-[2-[3-methoxy-4-[3-o-tolyl-ureido]-phenyl]-acetylamino]-phenyl}-cyclopentyl]-acetic acid tert-butyl ester (0.29 g, Reference Example 8) in a mixture of trifluoroacetic acid (7.5 mL), dichloromethane (1.5 mL) and water (1 mL) was stirred at room temperature for 1.5 hours and then evaporated. The residue was chased with toluene to yield a green glass, which was subjected to preparative HPLC [HyperPrep HS C-18 silica column using methanol with 0.05% trifluoroacetic acid and water with 0.05% trifluoroacetic acid as the mobile phase] to give the title compound (0.05 g) as a white solid, m.p. 223–226° C. LC-MS: RT=3.51 minutes, MS(ES+): 538(M+Na+), 516(M+H)+, 554(M+K)+; MS(ES−): 514(M−H)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07166616B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-d292e60bece9461fbfafe6f701aae314 |
| Source note | uspto-grants-2007_01 |