Potassium Carbonate → HCID 178418772, 화합물

HRID 635888

반응식

HRID 635888 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][C:10]([O:12]CC)=O)=[CH:4][CH:3]=1.Cl.[C:17]([NH2:20])(=[NH:19])[CH3:18].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[C:10]([OH:12])[N:20]=[C:17]([CH3:18])[N:19]=2)=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 67170Acetamidine monohydrochlorideHCID 2758844Ethyl 3-(4-Fluorophenyl)-3-Oxopropanoate

생성물 1

HCID 178418772HCID 178418772, 화합물수율 63%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
65 °C

실험 절차

(Step 2) A mixture of 145 g of ethyl 3-(4-fluorophenyl)-3-oxopropionate, 97.8 g of acetamidine hydrochloride, 191 g of powdered potassium carbonate, and 1.16 L of ethanol was stirred at 60-70° C. for 16 hours. This reaction mixture was filtered to remove insolubles and the filtrate was concentrated. To the residue was added water and the resultant was neutralized with acetic acid. The crystals that separated out were collected by filtration, washed with water, and dried to provide 88.7 g of the title compound as white crystals. m.p. 290-292° C. (decomp.)

후처리

  1. filtrationThis reaction mixture was filtered
  2. customto remove insolubles
  3. concentrationthe filtrate was concentrated
  4. additionTo the residue was added water
  5. customThe crystals that separated out
  6. filtrationwere collected by filtration
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-066fe036f2d443f8863dc2f44abb0f3f
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06191149B1

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