Sodium Hydroxide → 2-(4-Fluorophenyl)-3-(pyridin-4-yl)-1H-pyrrole

HRID 1244987노트

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HRID 1244987 반응식
C(OC([C:6]1[C:7]([C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)=[C:8]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)[NH:9][CH:10]=1)=O)C.[OH-].[Na+]>C(O)(=O)C.S(=O)(=O)(O)O.O>[F:17][C:14]1[CH:13]=[CH:12][C:11]([C:8]2[NH:9][CH:10]=[CH:6][C:7]=2[C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)=[CH:16][CH:15]=1

참가 물질

6

반응물 2

HCID 14798Sodium HydroxideHCID 219228384-Ethoxycarbonyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)-1H-pyrrole

생성물 1

HCID 219226632-(4-Fluorophenyl)-3-(pyridin-4-yl)-1H-pyrrole수율 99.1%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매HCID 1118Sulfuric Acid용매

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온도
100 °C

실험 절차

15.00 g (48.3 mmol) of 4-ethoxycarbonyl-2-(4-fluorophenyl)-3-(pyridin-4-yl)-1H-pyrrole [prepared as described in Example 1(i) above] were dissolved in a mixture of 90 ml of acetic acid, 30 ml of sulfuric acid and 60 ml of water and the resulting solution was stirred at 100° C. for 16 hours. At the end of this time, the reaction mixture was cooled to room temperature and then made alkaline with a 10% aqueous solution of sodium hydroxide. The resulting mixture was extracted with ethyl acetate and the organic extract was washed with water, dried over anhydrous sodium sulfate and then concentrated by evaporation under reduced pressure to give 11.40 g (yield 99%) of the title compound as a pale red powder.

후처리

  1. temperatureAt the end of this time, the reaction mixture was cooled to room temperature
  2. extractionThe resulting mixture was extracted with ethyl acetate
  3. extractionthe organic extract
  4. washwas washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated by evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-07ba54922e084a65bbc777d68828996e
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07122666B2

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