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Chloroform → 2-Chloro-4-iodobenzylamine

HRID 551326
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HRID 551326 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[CH2:9][N:10]1C(=O)C2=CC=CC=C2C1=O.C(Cl)(Cl)Cl>C(O)C.O.NN>[Cl:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[CH2:9][NH2:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6212ChloroformHCID 66719866N-[(2-chloro-4-iodophenyl)methyl]phthalimide

생성물 1

HCID 671887782-Chloro-4-iodobenzylamine수율 143.5%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 24654Hydrazine hydrate (1:1)용매

반응 조건

온도
70 °C

실험 절차

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

In a solution of 2.9 g of N-[(2-chloro-4-iodophenyl)methyl]phthalimide in 60 mL of ethanol, 3.0 mL of 80% hydrazine monohydrate aqueous solution was added, and stirred at 70° C. for 30 minutes. After the completion of the reaction, the reaction mixture was left and cooled to room temperature, 100 mL of chloroform was added therein and insoluble substance was filtered off, and the solvent was distilled off under reduced pressure. The procedure comprising adding 30 mL of chloroform in the residue, filtering off insoluble material and distilling off the solvent under reduced pressure was repeated twice to obtain 2.8 g of the aimed product as yellow oily substance.

후처리

  1. customAfter the completion of the reaction
  2. waitthe reaction mixture was left
  3. temperaturecooled to room temperature
  4. filtrationinsoluble substance was filtered off
  5. distillationthe solvent was distilled off under reduced pressure
  6. additionThe procedure comprising adding 30 mL of chloroform in the residue
  7. filtrationfiltering off insoluble material
  8. distillationdistilling off the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-b266b9d6570a4cf398f60cc03f4b1d13
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07947715B2

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