2-(Benzo[d]isoxazol-3-yl)-2-bromoacetic acid → 1,2-Benzisoxazole, 3-(bromomethyl)-

HRID 1032328

Reaktionsgleichung

Reaktionsgleichung von HRID 1032328
[Br:1][CH:2]([C:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[O:8][N:7]=1)C(O)=O>C1(C)C=CC=CC=1>[Br:1][CH2:2][C:6]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[O:8][N:7]=1

Komponenten

3

Versuchsvorschrift

Alpha-bromo-1,2-benzisoxazole-3-acetic acid (58.0 g, 0.23 mole) is suspended in toluene (350 mL) and the mixture is stirred at reflux for 18 hours. The solvent is evaporated and the residue is taken up in methylene chloride (250 mL). This solution is washed with saturated aqueous sodium bicarbonate (2×50 mL), water (50 mL) and dried over anhydrous magnesium sulfate. The solution is filtered and evaporated to afford 3-bromomethyl-1,2-benzisoxazole, m.p. 60-62° C. The compound is purified by recrystallisation from ether-hexane, m.p. 64-66° C.

Aufarbeitung

  1. temperatureat reflux for 18 hours
  2. customThe solvent is evaporated
  3. washThis solution is washed with saturated aqueous sodium bicarbonate (2×50 mL), water (50 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe solution is filtered
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-95b70d12fc1848e985b9e964cfe75c47
Quelldatensatz
uspto-grants-1990_09
Patentnummer
US04957931

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