Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | 4-Methylcatechol | HCID 9958 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 1,3-Benzodioxole, 5-methyl- | HCID 81564 | 71,9% |
Reaktionsschritte
A mixture of 4-methylcatechol (26.0 g, 209.4 mmol) and NaOH (18.4 g, 461.0 mmol) in CH2Cl2 (40.0 mL) was heated to 100° C. under nitrogen for 2 hours. The solution was allowed to cool to ambient temperature and diluted with ethyl acetate (500 mL). The mixture was washed with NaHCO3 (200 mL) and H2O (2×200 mL). The organic layer was dried over Na2SO4, filtered and concentrated to give a crude oil. Flash chromatography eluting with hexane (100%) gradient to ether/hexane (1:1) afforded the title intermediate as a colorless oil 20.5 g (71.9%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US06605596B2 |
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| Quelldatensatz | uspto-grants-2003_08 |
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| ORD ID | ord-07f0cc7de98e4b4aa8fd7d1923e436ad |
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| Quellennotiz | uspto-grants-2003_08 |
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