Potassium Carbonate → HCID 178418772、化合物

HRID 8698

反応式

HRID 8698 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 178418772HCID 178418772、化合物収率 87.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-87d3e58ebd044febb2246a63639c98ea
出典データセット
uspto-grants-2006_08
特許番号
US07091206B2

関連ノート

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