Potassium Carbonate → HCID 178418772, 화합물

HRID 8698

반응식

HRID 8698 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+]>CO>[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 87.6%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

8.7 kg of ethyl 3-(4-fluorophenyl)-3-oxopropionate, 11.7 kg of acetoamidine hydrochloride and 28.6 kg of potassium carbonate were stirred for 5 hours at about 50° C. in 34.5 kg of methanol. Insolubles were separated from the reaction mixture and washed with methanol, and the mother liquor and the washing were combined with water and neutralized with an 18% aqueous solution of hydrochloric acid. After neutralization, the crystal was ripened by stirring under reflux for 4 hours, and the precipitated crystal was isolated by centrifugation, washed with water, dried to obtain 7.4 kg of the target compound as a white crystal.

후처리

  1. customInsolubles were separated from the reaction mixture
  2. washwashed with methanol
  3. temperatureunder reflux for 4 hours
  4. customthe precipitated crystal was isolated by centrifugation
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-87d3e58ebd044febb2246a63639c98ea
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091206B2

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