HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → tert-Butyl 3-{2-[3-(2-acetylaminoethyl)indol-1-yl]ethoxy}-4-{4-[3-(2-methoxybenzyloxy)propoxy]phenyl}piperidine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | N-Acetyltryptamine | HCID 70547 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Tert-butyl 4-{4-[3-(2-methoxybenzyloxy)propoxy]phenyl}-3-[2-(toluene-4-sulphonyloxy)ethoxy]piperidine-1-carboxylate | HCID 86609984 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | tert-Butyl 3-{2-[3-(2-acetylaminoethyl)indol-1-yl]ethoxy}-4-{4-[3-(2-methoxybenzyloxy)propoxy]phenyl}piperidine-1-carboxylate | HCID 68501498 | — |
Reaction Steps
A suspension of 0.20 g of tert-butyl 4-{4-[3-(2-methoxybenzyloxy)propoxy]phenyl}-3-[2-(toluene-4-sulphonyloxy)ethoxy]piperidine-1-carboxylate (Example 14b) and 0.067 g of N-[2-(1H-indol-3-yl)ethyl]acetamide in 7 ml of N,N-dimethylformamide is admixed at 0° C. with 0.024 g of sodium hydride dispersion (60%) and stirred at room temperature over 20 hours. The reaction mixture is poured onto saturated aqueous sodium bicarbonate solution and extracted with ethyl acetate (2×). The combined organic phases are washed with brine, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained as a yellow oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.35 (EtOAc); Rt=5.69.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07842688B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-0fb41553436545509cd2e817fed0846f |
| Source note | uspto-grants-2010_11 |