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Potassium Cyanide → 2,5-Dichlorobenzyl cyanide

HRID 2043716
ノート
印刷プレビュー

反応式

HRID 2043716 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][C:7]([Cl:10])=[CH:6][C:3]=1[CH2:4]Br.[C-:11]#[N:12].[K+]>C(O)C.O>[Cl:1][C:2]1[CH:9]=[CH:8][C:7]([Cl:10])=[CH:6][C:3]=1[CH2:4][C:11]#[N:12]
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 9032Potassium CyanideHCID 34957442,5-Dichlorobenzyl bromide

生成物 1

HCID 35312002,5-Dichlorobenzyl cyanide収率 83.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

A mixture of 2,5-dichlorobenzyl bromide (5.4 g, 22.5 mmol) in 16 mL of ethanol and potassium cyanide (1.63 g, 25 mmol) in 4 mL of water was heated at 80° C. overnight, then cooled, and the solids were filtered and washed with ethanol to give 3.5 g of 2,5-dichlorophenylacetonitrile as a white powder melting at 89-91° C. The nitrile was suspended in 20 red, of ethanol, and 20 mL of a 25% aqueous NaOH solution was added. The mixture was heated in a CEM Explore™ microwave reactor at 140° C. for 30 minutes, then cooled, poured into ice water and acidified to pH 1 with concentrated HCl to give a precipitate. The precipitate was filtered, washed with water and dried in a vacuum oven at 90° C. for 5 h to give the title compound as a white powder.

後処理

  1. temperaturecooled
  2. filtrationthe solids were filtered
  3. washwashed with ethanol

出典と根拠

ORDレコード
ord-1650e19846b54c33875d992443f0bb64
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08586611B2

反応ノート

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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