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Sodium periodate → 3-Chloro-4-formylbenzonitrile

HRID 2090198
ノート
印刷プレビュー

反応式

HRID 2090198 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH:10]=CN(C)C)[C:5]#[N:6].I([O-])(=O)(=O)=[O:16].[Na+]>C1COCC1.O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[CH:10]=[O:16])[C:5]#[N:6]
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 2

HCID 23667635Sodium periodateHCID 873920413-Chloro-4-[2-(dimethylamino)vinyl]benzonitrile

生成物 1

HCID 122905503-Chloro-4-formylbenzonitrile

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

The crude 3-chloro-4-[2-(dimethylamino)vinyl]benzonitrile obtained in this way is taken up in 500 ml of THF/water (1:1), and 77.6 g (362.9 mmol) of sodium periodate are added. The mixture is stirred at room temperature for 18 h, and then the precipitate which has separated out is removed by filtration. The filtrate is mixed with saturated sodium bicarbonate solution and extracted three times with ethyl acetate. The combined organic phases are dried with sodium sulfate, and the solvent is removed in a rotary evaporator. The crude product is purified by column chromatography (silica gel, mobile phase: cyclohexane/ethyl acetate 7:3). 3.0 g (15% of theory) of the title compound are obtained.

後処理

  1. customthe precipitate which has separated out
  2. customis removed by filtration
  3. additionThe filtrate is mixed with saturated sodium bicarbonate solution
  4. extractionextracted three times with ethyl acetate
  5. dry with materialThe combined organic phases are dried with sodium sulfate
  6. customthe solvent is removed in a rotary evaporator
  7. customThe crude product is purified by column chromatography (silica gel, mobile phase: cyclohexane/ethyl acetate 7:3)

出典と根拠

ORDレコード
ord-d16e1e8c34f34d2a94c5d8ca2434f704
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436180B2

反応ノート

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