HuagongsheHuagongshe Chemistry Print Report · For research reference only
O-Phenylenediamine → (RS)-1-[2-(1H-benzoimidazol-2-ylmethyl)-piperidin-1-yl]-1-[5-(4-fluoro phenyl)-2-methyl-thiazol-4-yl]-methanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | O-Phenylenediamine | HCID 7243 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | (1-{1-[5-(4-Fluoro-phenyl)-2-methyl-thiazol-4-yl]-methanoyl}-piperidin-2-yl)-acetic acid | HCID 23146320 | — |
| Product | (RS)-1-[2-(1H-benzoimidazol-2-ylmethyl)-piperidin-1-yl]-1-[5-(4-fluoro phenyl)-2-methyl-thiazol-4-yl]-methanone | HCID 17973686 | 52% |
Reaction Steps
(RS)-(1-{1-[5-(4-Fluoro-phenyl)-2-methyl-thiazol-4-yl]-methanoyl}-piperidin-2-yl)-acetic acid, D17 (110 mg, 0.3 mmol) and benzene-1,2-diamine (33 mg, 0.3 mmol) in PPA (2 g) were heated at 140° C. for 3.5 h. The cooled reaction mixture was poured onto a mixture of crushed ice and K2CO3. The basic aqueous solution was extracted with ethyl acetate (3×). The combined organics were washed with brine, dried (MgSO4) and the solvent removed in vacuo. Chromatography (silica gel, ethyl acetate) afforded the title compound as a dark yellow gum (72 mg, 52%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897618B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-d731b6c5bd434cd5811acee81bcb7cd3 |
| Source note | uspto-grants-2011_03 |