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

HRID 1032328ノート

反応式

HRID 1032328 の反応式
[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

参加物

3

反応物 1

HCID 129470982-(Benzo[d]isoxazol-3-yl)-2-bromoacetic acid

生成物 1

HCID 34991891,2-Benzisoxazole, 3-(bromomethyl)-

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-95b70d12fc1848e985b9e964cfe75c47
出典データセット
uspto-grants-1990_09
特許番号
US04957931

反応ノート

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