Potassium Carbonate → 1-(o-Fluorobenzyl)-2[(di-sec-butylamino)acetyl]pyrrole

HRID 437051

반응식

HRID 437051 반응식
Cl[CH2:2][C:3]([C:5]1[N:6]([CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[F:17])[CH:7]=[CH:8][CH:9]=1)=[O:4].[CH:18]([NH:22][CH:23]([CH2:25][CH3:26])[CH3:24])([CH2:20][CH3:21])[CH3:19].C(=O)([O-])[O-].[K+].[K+]>C1(C)C(C)=CC=CC=1.CCOCC>[F:17][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[CH2:10][N:6]1[CH:7]=[CH:8][CH:9]=[C:5]1[C:3](=[O:4])[CH2:2][N:22]([CH:23]([CH2:25][CH3:26])[CH3:24])[CH:18]([CH2:20][CH3:21])[CH3:19]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 12277DI-Sec-butylamineHCID 203915312-Chloro-1-{1-[(2-fluorophenyl)methyl]-1H-pyrrol-2-yl}ethan-1-one

생성물 1

HCID 203915581-(o-Fluorobenzyl)-2[(di-sec-butylamino)acetyl]pyrrole

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 7237O-Xylene용매

반응 조건

온도
120 °C

실험 절차

A mixture of 16.0 g of 2-chloroacetyl-1-(o-fluorobenzyl)pyrrole, Example 1a, 8.3 g of di-sec-butylamine and 20.0 g of potassium carbonate in 250 ml xylene is stirred at 120° C. for 72 hours. The mixture is cooled, washed with water, dried and filtered and the xylene is evaporated leaving a brown oil. The oil is dissolved in ether and extracted into a 2N hydrogen chloride solution. The aqueous acidic solution is basified with a sodium carbonate solution and extracted with ether. The ether solution is washed, dried and filtered and the ether removed leaving a brown oil of 1-(o-fluorobenzyl)-2[(di-sec-butylamino)acetyl]pyrrole. Infrared and nuclear magnetic resonance spectra confirm this structure.

후처리

  1. temperatureThe mixture is cooled
  2. washwashed with water
  3. customdried
  4. filtrationfiltered
  5. customthe xylene is evaporated
  6. customleaving a brown oil
  7. extractionextracted into a 2N hydrogen chloride solution
  8. extractionextracted with ether
  9. washThe ether solution is washed
  10. customdried
  11. filtrationfiltered
  12. customthe ether removed

출처 및 근거

ORD 기록
ord-4510cb9941db4bcf8af22680c94c132b
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04029672

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