HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178493279, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 178493280 | HCID 178493280 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178493279 | HCID 178493279 | 78% |
Reaction Steps
To a solution of trans-4-[{2-[({[4-({[tert-butyl(dimethyl)silyl]oxy}methyl)-2-chloro-5-methoxyphenyl]amino}carbonyl)oxy]ethyl}(methyl)amino]cyclohexyl hydroxy(di-2-thienyl)acetate (intermediate 61; 315 mg; 0.44 mmol) in 6 ml THF were added 1.31 ml (1.31 mmol) of aqueous 1M HCl and the system was stirred at room temperature for 2.5 hrs. The solution was basified with aqueous 4% sodium hydrogen carbonate solution and extracted thrice with ethyl acetate. The organic extracts were washed with brine, dried and concentrated. The residue was purified by preparative reversed-phase HPLC (CH2Cl2/isopropanol 10:0 to 9:1) to give 78% of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09315463B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-ffde776e00c24531ab02fdf4e3a86ffa |
| Source note | uspto-grants-2016_04 |