Chlorosuccinimide → 2-chloro-N,N-dimethyl-3-nitro-aniline

HRID 352462

反応式

HRID 352462 の反応式
[CH3:1][N:2]([CH3:12])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-:11])=[O:10])[CH:4]=1.[Cl:13]N1C(=O)CCC1=O>CN(C=O)C>[CH3:1][N:2]([CH3:12])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([N+:9]([O-:11])=[O:10])[C:4]=1[Cl:13]

参加物

4

反応物 2

HCID 31398ChlorosuccinimideHCID 69269N,N-Dimethyl-3-nitroaniline

生成物 1

HCID 227123482-chloro-N,N-dimethyl-3-nitro-aniline収率 101.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

25 g of N,N-dimethyl-3-nitroaniline is dissolved in 225 ml of DMF. 20 g of N-chlorosuccinimide dissolved in 190 ml of DMF is slowly added dropwise and the solution is stirred at RT. After 24 hours, the solvent is evaporated. About 500 ml of ice is added to the red residue. The suspension is extracted three times with about 200 ml of diethylether. The ether phases are dried over Na2SO4, filtered, and evaporated down. 30.4 g of N,N-dimethyl-2-chloro-3-nitroaniline is obtained as a red oil. The crude product is used further without any additional purification.

後処理

  1. additionis slowly added dropwise
  2. customthe solvent is evaporated
  3. additionAbout 500 ml of ice is added to the red residue
  4. extractionThe suspension is extracted three times with about 200 ml of diethylether
  5. dry with materialThe ether phases are dried over Na2SO4
  6. filtrationfiltered
  7. customevaporated down

出典と根拠

ORDレコード
ord-6ec2464b864f4df392236929417f9e8e
出典データセット
uspto-grants-2004_06
特許番号
US06747051B2

関連ノート

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