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5-Chloro-3,3-dibromo-1-ethyl-7-azaoxindole → HCID 18973025, 화합물

HRID 2394372
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HRID 2394372 반응식
[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
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참가 물질

4

반응물 1

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

생성물 1

HCID 18973025HCID 18973025, 화합물

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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%)

출처 및 근거

ORD 기록
ord-7f1c160c7e1b4b28b848b34c356f2b3d
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05811432

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