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Acetic Acid → 2-Amino-5-bromobenzophenone

HRID 463490
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HRID 463490 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6]([CH:16]=1)=[C:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[O:8][N:9]=2.C(O)(=O)C>[Zn].O>[NH2:9][C:5]1[CH:4]=[CH:3][C:2]([Br:1])=[CH:16][C:6]=1[C:7]([C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)=[O:8]
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참가 물질

5

반응물 2

HCID 176Acetic AcidHCID 3472905-Bromo-3-phenyl-2,1-benzisoxazole

생성물 1

HCID 996772-Amino-5-bromobenzophenone수율 94%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

5-Bromo-3-phenyl-2,1-benzisoxazole (7.5 g, 28.6 mmol), water (14.6 ml), and zinc dust (9.3 g, 143 mmol) were combined. Acetic acid (8.6 ml, 143 mmol) was added and the mixture was stirred and heated at 80° C. for 90 minutes. After cooling to room temperature, both the liquid and solid portion of the reaction were extracted with methylene chloride. The combined methylene chloride solutions was washed once with sodium hydroxide solution (10%) and several times with water. Drying (sodium sulfate) and evaporation yielded the desired product (7.42 g) of mp. 92°-102° C.

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionthe liquid and solid portion of the reaction were extracted with methylene chloride
  3. washThe combined methylene chloride solutions was washed once with sodium hydroxide solution (10%) and several times with water
  4. customDrying
  5. custom(sodium sulfate) and evaporation

출처 및 근거

ORD 기록
ord-b7e3e13aa1b94319bbd3a75180d2377c
출처 데이터셋
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04519937

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