Sodium Carbonate → HCID 19077476, Verbindung

HRID 964566

Reaktionsgleichung

Reaktionsgleichung von HRID 964566
[CH3:1][C:2]1[C:7]2[O:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[C:6]=2[CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[Br:21]Br>CCCCCC>[Br:21][C:3]1[CH:4]=[CH:5][C:6]2[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=3[O:8][C:7]=2[C:2]=1[CH3:1]

Komponenten

5

Edukt 3

HCID 10340Sodium CarbonateHCID 24408BromineHCID 43489Dibenzofuran, 4-methyl-

Produkt 1

HCID 19077476HCID 19077476, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8058HexaneLösungsmittel

Versuchsvorschrift

4-Methyldibenzofuran (30 g, 165 mmol) and sodium carbonate (17.5 g, 165 mmol) were mixed in hexane (300 ml) and bromine (26.4 g, 165 mmol) was added. The reaction was stirred at room temperature for 72 hours, then the solvent was removed in vacuo to give an oil which crystallised. Recrystallisation from IMS yielded several batches of off-white crystals (31.22 g, 72%) with m.p. 124°-125° C. (Found: C, 58.59; H, 3,28. C13H9BrO 0.31H2O requires: C, 58.58; H, 3.63%); δH [2H6 ]-DMSO 8.15 (1H, d), 7.9 (1H, d), 7.7 (1H, d), 7.4 (1H, t), 7.05 (2H, m), 2.6 (3H, s); m/z 260/262 (M+).

Aufarbeitung

  1. customthe solvent was removed in vacuo
  2. customto give an oil which
  3. customcrystallised
  4. customRecrystallisation from IMS yielded several batches of off-white crystals (31.22 g, 72%) with m.p. 124°-125° C. (Found: C, 58.59; H, 3,28. C13H9BrO 0.31H2O requires: C, 58.58; H, 3.63%)

Quellen und Nachweise

ORD-Eintrag
ord-371d0e347a4640b38d6a9dc5fcac741b
Quelldatensatz
uspto-grants-1998_06
Patentnummer
US05770598

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