p-Fluorophenethylamine → 2-Chloro-N-[2-(4-fluoro-phenyl)-ethyl]-acetamide

HRID 2265922ノート

反応式

HRID 2265922 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][NH2:10])=[CH:4][CH:3]=1.CCN(C(C)C)C(C)C.[Cl:20][CH2:21][C:22](Cl)=[O:23]>C1COCC1>[Cl:20][CH2:21][C:22]([NH:10][CH2:9][CH2:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1)=[O:23]

参加物

5

反応物 3

HCID 4653p-FluorophenethylamineHCID 6577Chloroacetyl chlorideHCID 81531Diisopropylethylamine

生成物 1

HCID 23845922-Chloro-N-[2-(4-fluoro-phenyl)-ethyl]-acetamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of 4-fluorophenylethylamine (1.0 equivalent) in dried THF was added Hunig's base (DIEA) (1 equivalent). The mixture was then stirred for 3 minutes at 0° C. Thereafter, a solution of chloroacetylchloride (1.0 equivalent) in THF was added via a syringe over a period of 7 minutes. The reaction mixture was then stirred at room temperature for 1 hour after which time the reaction mixture was condensed in vacuo, quenched with water, extracted with ethyl acetate (3×) and dried over Na2SO4. After concentration in vacuo, compound 1 shown above was obtained, which was carried on further without further purification. LC/MS=M+H 216.1 at 2.18 minutes.

後処理

  1. stirringThe reaction mixture was then stirred at room temperature for 1 hour after which time the reaction mixture
  2. customcondensed in vacuo
  3. customquenched with water
  4. extractionextracted with ethyl acetate (3×)
  5. dry with materialdried over Na2SO4
  6. concentrationAfter concentration in vacuo, compound 1
  7. customabove was obtained
  8. customfurther without further purification
  9. waitLC/MS=M+H 216.1 at 2.18 minutes

出典と根拠

ORDレコード
ord-38008694e1d74b03ba67e67dbb531d89
出典データセット
uspto-grants-2010_12
特許番号
US07858631B2

反応ノート

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