2-Fluoroaniline → HCID 18183268、化合物

HRID 1018899ノート

反応式

HRID 1018899 の反応式
[Br:1][CH:2]([CH3:6])[C:3](O)=[O:4].[F:7][C:8]1[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=1[NH2:10].[CH:15]1(N=C=NC2CCCCC2)CCCCC1>C(Cl)(Cl)Cl>[F:7][C:8]1[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=1[N:10]([CH3:15])[C:3](=[O:4])[CH:2]([Br:1])[CH3:6]

参加物

5

反応物 3

HCID 95842-FluoroanilineHCID 10868DicyclohexylcarbodiimideHCID 117292-Bromopropionic acid

生成物 1

HCID 18183268HCID 18183268、化合物収率 87.4%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

反応条件

温度
0 °C

実験手順

2-Bromopropionic acid(3.4 g, 0.022 mol) and 2-fluoroaniline(3 g, 0.024 mol) were dissolved in 50 ml of chloroform and cooled to 0° C. A solution of dicyclohexylcarbodiimide(5 g, 0.024 mol) in 10 ml of chloroform was slowly injected through a syringe. A temperature of the reaction mixture was raised to room temperature and it was stirred for 1 hour. Solid remained during the reaction was filtered out and washed twice with 20 ml of chloroform. The filtrate was concentrated under reduced pressure and the crude product was purified by column chromatography (eluent; ethyl acetate/n-hexane=1/3) to afford 5 g of the target product.

後処理

  1. temperatureA temperature of the reaction mixture was raised to room temperature
  2. filtrationwas filtered out
  3. washwashed twice with 20 ml of chloroform
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe crude product was purified by column chromatography (eluent; ethyl acetate/n-hexane=1/3)

出典と根拠

ORDレコード
ord-81ded47ad5b04d66ab9d4db4deeb5d12
出典データセット
uspto-grants-2002_11
特許番号
US06486098B1

反応ノート

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