2-Chloro-4-nitrotoluene → (E)-2-(2-chloro-4-nitrophenyl)-N,N-dimethylethenamine

HRID 735124

反応式

HRID 735124 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[CH3:11].C(O[CH:17](N(C)C)[N:18]([CH3:20])[CH3:19])(C)(C)C>C1COCC1>[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1/[CH:11]=[CH:17]/[N:18]([CH3:20])[CH3:19]

参加物

4

反応物 2

HCID 84912-Chloro-4-nitrotolueneHCID 79885tert-Butoxy bis(dimethylamino)methane

生成物 1

HCID 11310699(E)-2-(2-chloro-4-nitrophenyl)-N,N-dimethylethenamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A reaction mixture of 8.49 g (48 mmol) of 2-chloro-4-nitrotoluene and 15.03 mL (72.8 mmol) of tert-butoxybis(dimethylamino)methane in 200 mL of THF is refluxed for 8 hours. The reaction solution is evaporated down and the residue is combined with petroleum ether. The precipitate is filtered off, rinsed with petroleum ether and dried at ambient temperature under a high vacuum. The product is used in other reactions without further purification. Yield: 11 g, C10H11ClN2O2 (M=226.66); calc.: molecular ion peak (M+H)+: 227/229; found: molecular ion peak (M+H)+: 227/229; Rf value: 0.55 (silica gel, petroleum ether/ethyl acetate (3:1)).

後処理

  1. temperatureis refluxed for 8 hours
  2. customThe reaction solution is evaporated down
  3. filtrationThe precipitate is filtered off
  4. washrinsed with petroleum ether
  5. customdried at ambient temperature under a high vacuum
  6. customThe product is used in other reactions without further purification

出典と根拠

ORDレコード
ord-9e3147b35d304049baf7b8b39ffd3b4b
出典データセット
uspto-grants-2009_09
特許番号
US07592373B2

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