2-Methyl-5-Nitroaniline → (2-Methyl-5-nitrophenyl)pyrrolidine

HRID 2070341

反応式

HRID 2070341 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[NH2:11].C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH:20](Br)[CH2:21][CH3:22]>CN(C)C=O>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[N:11]1[CH2:22][CH2:21][CH2:20][CH2:19]1

参加物

5

反応物 3

HCID 74442-Methyl-5-NitroanilineHCID 107921,2-DibromobutaneHCID 11430Potassium Carbonate

生成物 1

HCID 69558510(2-Methyl-5-nitrophenyl)pyrrolidine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

To the mixture containing 2-methyl-5-nitrophenylamine and potassium carbonate (4 eq) in dimethyl formamide was added 1,2 dibromobutane (4 eq) and the resulting mixture was stirred at 70° C. for 16 hours. The reaction mixture was then concentrated and partitioned between ethyl acetate and water. The organic layer was dried with sodium sulfate and concentrated and purified on silica gel to give (2-methyl-5-nitrophenyl)pyrrolidine.

後処理

  1. concentrationThe reaction mixture was then concentrated
  2. custompartitioned between ethyl acetate and water
  3. dry with materialThe organic layer was dried with sodium sulfate
  4. concentrationconcentrated
  5. custompurified on silica gel

出典と根拠

ORDレコード
ord-94369907dd7b4e7a88b5b3955fb666d3
出典データセット
uspto-grants-2012_10
特許番号
US08299108B2

関連ノート

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