HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 22248819, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 69596297 | HCID 69596297 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22248819 | HCID 22248819 | 121.7% |
Reaction Steps
To a solution of 4-{4-[1-(2-chloro-phenyl)-ethoxy]-pyrimidin-2-yl}-piperazine-1-carboxylic acid tert-butyl ester (I-2b) (64.3 mg, 0.15 mmol) in 2.0 mL of dichloromethane was added trifluoroacetic acid (177.4 μL, 2.30 mmol) and the mixture was stirred for 1.5 h at ambient temperature. The reaction was concentrated, and the residue dissolved in 1 M HCl(aq) (10 mL). This was extracted with ethyl acetate (10 mL), separated, and the aqueous layer was adjusted to a pH of 12 using 5 M KOH(aq). This aqueous mixture was extracted with ethyl acetate (2×15 mL) and the combined organic extracts were dried over sodium sulfate and concentrated to give 58.2 mg of the title product (2-A).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06995159B2 |
| Source dataset | uspto-grants-2006_02 |
| ORD ID | ord-ff2c4bc2b8be4f188e396a1a132a7919 |
| Source note | uspto-grants-2006_02 |