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

HRID 1032328노트

반응식

HRID 1032328 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-95b70d12fc1848e985b9e964cfe75c47
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04957931

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