HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dichloromethane → HCID 60169549, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | Propylphosphonic anhydride | HCID 111923 | — |
| Edukt | 5-Methyl-2-(pyrimidin-2-yl)benzoic acid | HCID 44517264 | — |
| Edukt | (S)-1-Boc-4-oxopiperidine-2-carboxylic acid tert-butylamine salt | HCID 66848353 | — |
| Produkt | HCID 60169549 | HCID 60169549 | — |
Reaktionsschritte
Alternatively Compound 13 was obtained by the following procedure: 5-methyl-2-(pyrimidin-2-yl)benzoic acid (428 mg, 2 mmol; prepared according to WO 2008147518), intermediate 34 (500 mg, 2 mmol) and DIPEA (0.65 ml) were dissolved in DCM (5 ml) at 0° C., then T3P (50% in DCM, 1.5 g) was added. The mixture is stirred at reflux for 8 hours then at RT overnight. The reaction was washed with NaOH 1M and water, dried (Na2SO4) and evaporated. The crude was purified by silica gel column chromatography (DCM to DCM/MeOH=95/05). 180 mg of the desired compound were isolated.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08859608B2 |
| Quelldatensatz | uspto-grants-2014_10 |
| ORD ID | ord-b24d643e62b54fb8942e4316b1d777d7 |
| Quellennotiz | uspto-grants-2014_10 |