HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
beta-Bromostyrene → 1-Methyl-2-styryl-2-hydroxy-6-piperidone
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | beta-Bromostyrene | HCID 7667 | — |
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | 2,6-Piperidinedione, 1-methyl- | HCID 161476 | — |
| Edukt | Magnesium | HCID 5462224 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 1-Methyl-2-styryl-2-hydroxy-6-piperidone | HCID 53776161 | — |
Reaktionsschritte
The Grignard reagent prepared in 300 ml of THF from 24 g (1.0 mole) of magnesium and 42 g (0.30 mole) of β-bromostyrene is decanted from excess metal and added dropwise under nitrogen to a solution of 27 g (0.21 moles) of N-methyl glutarimide at 3°- 5°. After 11/2 hrs. at room temperature, the mixture is treated with 250 ml of saturated NH4Cl solution with cooling. The separated aqueous layer is reextracted and the combined THF extracts washed with salt, dried over MgSO4 and freed of solvent. Product is extracted into hot ether and crystallized on cooling to yield white crystals, mp 108°- 112° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04038273 |
| Quelldatensatz | uspto-grants-1977_07 |
| ORD ID | ord-ecfd5e6d54e74309bff4d1113272e89d |
| Quellennotiz | uspto-grants-1977_07 |