HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → HCID 66750860, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| Edukt | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | Methyl 4-(2-aminoethyl)benzoate hydrochloride | HCID 13078671 | — |
| Edukt | HCID 66750854 | HCID 66750854 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | HCID 66750860 | HCID 66750860 | 71,5% |
Reaktionsschritte
A mixture of 2-[4-(2-tert-butylphenyl)piperazin-1-yl]-2-oxoacetic acid (Example 44, 1.0 g, 3.44 mmol), methyl 4-(2-aminoethyl)benzoate hydrochloride (0.83 g, 4.13 mmol), triethylamine (0.72 mL, 5.16 mmol), EDCI (0.64 g, 4.13 mmol) and HOBt (0.63 g, 4.13 mmol) in N,N-dimethylformamide (10 mL) was stirred at room temperature for 16 h. The reaction mixture was poured into saturated NaHCO3 solution and extracted with ethyl acetate. The extract was washed with saturated NaHCO3 solution and brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate 80:20 to 34:66) to give the title compound (1.11 g, 71%) as a white amorphous.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08853215B2 |
| Quelldatensatz | uspto-grants-2014_10 |
| ORD ID | ord-375f6e52ea0e48eca00b0610d81ad806 |
| Quellennotiz | uspto-grants-2014_10 |