2-(4-Chloro-phenyl)-N-ethyl-acetamide → [2-(4-Chloro-phenyl)-ethyl]-ethyl-amine hydrochloride

HRID 1866529ノート

反応式

HRID 1866529 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([NH:11][CH2:12][CH3:13])=O)=[CH:4][CH:3]=1>O1CCCC1.CO.Cl>[ClH:1].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH2:9][NH:11][CH2:12][CH3:13])=[CH:6][CH:7]=1

参加物

5

反応物 1

HCID 44191372-(4-Chloro-phenyl)-N-ethyl-acetamide

生成物 1

HCID 69026677[2-(4-Chloro-phenyl)-ethyl]-ethyl-amine hydrochloride収率 99%

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 2-(4-chloro-phenyl)-N-ethyl-acetamide (preparation 80), (437 mg, 2.22 mmol) and borane tetrahydrofuran complex (1M, 8.88 mL, 8.88 mmol) in tetrahydrofuran was heated under reflux for 18 hours. The cooled reaction mixture was then diluted with methanol (5 mL) and 12M hydrochloric acid (2 mL) and the re-heated to reflux for a further hour. The mixture was cooled to room temperature and concentrated in vacuo. Trituration of the residue with ethyl acetate afforded the title compound as a colourless solid in 99% yield, 403 mg.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. customThe cooled reaction mixture
  4. temperaturethe re-heated
  5. temperatureto reflux for a further hour
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9498db197f2140f3872caad7c4f9cd19
出典データセット
uspto-grants-2009_12
特許番号
US07629358B2

反応ノート

読み込み中…