HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetyl chloride → N'-acetyl-2,2-dimethylpropanohydrazide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetyl chloride | HCID 6367 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 2,2-Dimethylpropanehydrazide | HCID 545147 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | N'-acetyl-2,2-dimethylpropanohydrazide | HCID 23525705 | — |
Reaktionsschritte
To a mixture of 2,2-dimethyl-propionic acid hydrazide (2.32 g, 20 mmol), sodium bicarbonate (1.68 g, 20 mmol) in tetrahydrofuran and water (1:1, 40 mL) was added acetyl chloride (1.56 g, 20 mmol) dropwise. The mixture was stirred overnight and concentrated in vacuo. The residue was extracted with dichloromethane and isopropyl alcohol (10:1) (3×10 mL). The organic extracts were combined, dried over MgSO4 and concentrated to give a white solid. The solid was recrystallized from tetrahydrofuran and hexane (1:8) to provide the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm 1.11-1.14 (m, 9 H) 1.83 (s, 3 H) 9.28 (br s, 1 H) 9.53 (br s, 1 H); MS (ESI) m/z 159 (M+H)+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08481574B2 |
| Quelldatensatz | uspto-grants-2013_07 |
| ORD ID | ord-66bee90cb8ed40fa841c72b09adb1271 |
| Quellennotiz | uspto-grants-2013_07 |