Ethyl Acetate → 2-Chloro-4-methylbenzonitrile

HRID 1172674

反応式

HRID 1172674 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[Cl:9].[Cu][C:11]#[N:12].C(OCC)(=O)C>CN(C)C=O>[Cl:9][C:3]1[CH:4]=[C:5]([CH3:8])[CH:6]=[CH:7][C:2]=1[C:11]#[N:12]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 1387894-Bromo-3-chlorotolueneHCID 178418546HCID 178418546、化合物

生成物 1

HCID 3194752-Chloro-4-methylbenzonitrile収率 93.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

25.0 g 4-bromo-3-chlorotoluene and 21.8 g copper (I) cyanide were dissolved in 200 ml dimethylformamide and stirred at 150° C. for three hours. The cooled reaction mixture was diluted by addition of 300 ml ethyl acetate and washed three times with portions of 150 ml saturated NH4Cl solution. The precipitates were filtered off and the filtrate dried over MgSO4 and then reduced in vacuo to obtain 17.3 g 2-Chloro-4-methyl-benzonitrile. This material was used without purification in the next step.

後処理

  1. customThe cooled reaction mixture
  2. washwashed three times with portions of 150 ml saturated NH4Cl solution
  3. filtrationThe precipitates were filtered off
  4. dry with materialthe filtrate dried over MgSO4

出典と根拠

ORDレコード
ord-7d56b42e5602451ba9f5a80875b098d2
出典データセット
uspto-grants-2010_11
特許番号
US07834030B2

関連ノート

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