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Chloroform → 2-Chloro-4-iodobenzylamine

HRID 885812
ノート
印刷プレビュー

反応式

HRID 885812 の反応式
[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]
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 6212ChloroformHCID 66719866N-[(2-chloro-4-iodophenyl)methyl]phthalimide

生成物 1

HCID 671887782-Chloro-4-iodobenzylamine収率 143.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 24654Hydrazine hydrate (1:1)溶媒

反応条件

温度
70 °C

実験手順

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

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.

後処理

  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

出典と根拠

ORDレコード
ord-6bdf7e3d20a4430983c1672ebbf02d1e
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08242283B2

反応ノート

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