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5-Chloro-3,3-dibromo-1-ethyl-7-azaoxindole → HCID 18973025、化合物

HRID 2394372
ノート
印刷プレビュー

反応式

HRID 2394372 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[N:9][CH:10]=1)[N:7]([CH2:11][CH3:12])[C:6](=[O:13])[C:5]2(Br)Br>C(O)(=O)C.[Zn]>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[N:9][CH:10]=1)[N:7]([CH2:11][CH3:12])[C:6](=[O:13])[CH2:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 189730905-Chloro-3,3-dibromo-1-ethyl-7-azaoxindole

生成物 1

HCID 18973025HCID 18973025、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

実験手順

To a solution of 5-chloro-3,3-dibromo-1-ethyl-7-azaoxindole (4.60 g, 13.0 mmol) in glacial acetic acid (75 mL) was added, in portions, zinc powder (2.5 g, 39 mmol). An exothermic reaction took place immediately, however, stirring at room temperature was continued for 1 hour. The mixture was poured into ice/water and then extracted with ethyl acetate. The organic extract was washed with water, dried over magnesium sulfate and evaporated to leave an oil which was chromatographed on a column of silica gel eluting with chloroform. Fractions containing the desired product were combined and concentrated in vacuo to afford an off-white solid, 1.70 g (68%). M.p. 78°-82° C.

後処理

  1. customAn exothermic reaction
  2. extractionextracted with ethyl acetate
  3. extractionThe organic extract
  4. washwas washed with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. customto leave an oil which
  8. customwas chromatographed on a column of silica gel eluting with chloroform
  9. additionFractions containing the desired product
  10. concentrationconcentrated in vacuo
  11. customto afford an off-white solid, 1.70 g (68%)

出典と根拠

ORDレコード
ord-7f1c160c7e1b4b28b848b34c356f2b3d
出典データセット
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05811432

反応ノート

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