Potassium Carbonate → HCID 178418772、化合物

HRID 635888

反応式

HRID 635888 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+]>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

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 63%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
65 °C

実験手順

(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.)

後処理

  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

出典と根拠

ORDレコード
ord-066fe036f2d443f8863dc2f44abb0f3f
出典データセット
uspto-grants-2001_02
特許番号
US06191149B1

関連ノート

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