Water → N,N-Dibutyl-3-methoxybenzenamine

HRID 85321

반응식

HRID 85321 반응식
[CH2:1]([N:5]([CH2:13][CH2:14][CH2:15][CH3:16])[C:6]1[CH:7]=[C:8]([OH:12])[CH:9]=[CH:10][CH:11]=1)[CH2:2][CH2:3][CH3:4].CI.[C:19](=O)([O-])[O-].[K+].[K+].O>CN1CCCC1=O.C(OCC)(=O)C>[CH2:1]([N:5]([CH2:13][CH2:14][CH2:15][CH3:16])[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH3:19])[CH:7]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 601234N,N-Dibutyl-3-aminophenol

생성물 1

HCID 4068285N,N-Dibutyl-3-methoxybenzenamine수율 48.7%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
60 °C

실험 절차

In 70 ml of 1-methyl-2-pyrrolidone were dissolved 10.0 g (45.18 mmol) of 3-(dibutylamino)phenol and 12.8 g (90.18 mmol) of methyl iodide. To this mixture was added 18.7 g (135.3 mmol) of anhydrous potassium carbonate and the mixture was stirred with heating at 60° C. for 6 hours. After the reaction mixture was poured into 350 ml of water, extraction with ethyl acetate, washing with a saturated saline solution, drying over anhydrous sodium sulfate, and concentration were performed. The residue was purified by silica gel column chromatography to give 5.2 g of a colorless oily matter (yield: 48.7%).

후처리

  1. washwashing with a saturated saline solution
  2. dry with materialdrying over anhydrous sodium sulfate, and concentration
  3. customThe residue was purified by silica gel column chromatography
  4. customto give 5.2 g of a colorless oily matter (yield: 48.7%)

출처 및 근거

ORD 기록
ord-6b6196217cdd4cb797549516ead8b597
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846955B2

연결된 노트

불러오는 중…