HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 11775533, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Trimethylsilyl iodide | HCID 85247 | — |
| Reactant | HCID 60003257 | HCID 60003257 | — |
| Solvent | 1-Propanol | HCID 1031 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 11775533 | HCID 11775533 | 87% |
Reaction Steps
4-(4-Fluorophenyl)-2-(1-ethoxycarbonylpiperidin-4-yl)-5-(2-(1-(S)-phenylethyl)amino-4-pyrimidinyl)thiazole (2.4 g 4.5 mmol) was dissolved in CHCl3 (45 ml) and treated with Me3SiI (1.8 ml 13.5 mmol) at 60° C. for 6 h. The reaction mixture was combined with 6M HCl in propanol (18.5 ml), homogenized by vigorous stirring, poured on 2N NaOH and extracted twice with CH2Cl2. The combined organic phases were dried over Na2SO4, filtered, evaporated to dryness and purified by SiO2 chromatography (tert.butyl methyl ether/MeOH/NH3conc. 95/4.5/0.5 to 80/18/2) to yield the title compound (1.8 g 87%) as a white foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06608072B1 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-d3c1b71762ce424ca58789782d315330 |
| Source note | uspto-grants-2003_08 |