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Acetic Acid → 2-Amino-5-bromobenzophenone

HRID 463490
ノート
印刷プレビュー

反応式

HRID 463490 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

HCID 996772-Amino-5-bromobenzophenone収率 94%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b7e3e13aa1b94319bbd3a75180d2377c
出典データセット
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04519937

反応ノート

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