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

HRID 2070341

반응식

HRID 2070341 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-94369907dd7b4e7a88b5b3955fb666d3
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299108B2

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