Potassium Carbonate → 4-[2-(Diethylamino)ethoxy]benzonitrile

HRID 1858219

반응식

HRID 1858219 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1)#[N:2].[OH-].[Na+].C(=O)([O-])[O-].[K+].[K+].Cl.[CH2:19]([N:21]([CH2:25][CH3:26])[CH2:22][CH2:23]Cl)[CH3:20]>C1(C)C(C)=CC=CC=1.O>[CH2:19]([N:21]([CH2:25][CH3:26])[CH2:22][CH2:23][O:9][C:6]1[CH:7]=[CH:8][C:3]([C:1]#[N:2])=[CH:4][CH:5]=1)[CH3:20]

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 130194-CyanophenolHCID 133631-Chloro-2-(diethylamine)ethane hydrochlorideHCID 14798Sodium Hydroxide

생성물 1

HCID 3410044-[2-(Diethylamino)ethoxy]benzonitrile수율 74.7%

시약·촉매·용매 2

HCID 962Water용매HCID 7237O-Xylene용매

실험 절차

A solution of 8.04 g (67 mmol) of 4-cyanophenol in 100 ml of xylene was treated with a solution of 2.99 g (74 mmol) of sodium hydroxide in 20 ml of water and the mixture was stirred for 30 minutes. To this mixture were added 13.88 g (100 mmol) of potassium carbonate and 12.83 g (75 mmol) of 2-diethylaminoethyl chloride hydrochloride. The resulting mixture was then heated at reflux for 3 hours, subsequently left to cool, washed twice with 50 ml of water each time, dried over magnesium sulfate, filtered and evaporated to give 10.93 g (74%) of 4-(2-diethylaminoethoxy)benzonitrile as a colorless mobile liquid.

후처리

  1. temperatureThe resulting mixture was then heated
  2. temperatureat reflux for 3 hours
  3. waitsubsequently left
  4. temperatureto cool
  5. washwashed twice with 50 ml of water each time
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-7f3cb291a2d5419696549231206e08b8
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06150373

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