Aluminium lithium hydride → 3-(Aminomethyl)-2,6-dichloro-5-fluoroaniline

HRID 450331ノート

反応式

HRID 450331 の反応式
[Cl:1][C:2]1[C:10]([NH2:11])=[C:9]([Cl:12])[C:8]([F:13])=[CH:7][C:3]=1[C:4]([NH2:6])=O.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[NH2:11][C:10]1[C:2]([Cl:1])=[C:3]([CH:7]=[C:8]([F:13])[C:9]=1[Cl:12])[CH2:4][NH2:6]

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 866744963-Amino-2,4-dichloro-5-fluorobenzamide

生成物 1

HCID 825077343-(Aminomethyl)-2,6-dichloro-5-fluoroaniline

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

2,4-Dichloro-5-fluoro-3 amino-benzamide (6.00 g, 26.9 mmol) in THF (175 mL) is added dropwise to LiAlH4 (1 M in THF, 28.0 mL) in THF (175 mL). The reaction mixture is stirred for 1 h at rt and 5 h at reflux. Excess LiAlH4 is destroyed under cooling as described by L. F. Fieser & M. Fieser Vol 1, p 584 Wiley 1967. After 30 min the mixture is filtered, the filtrate is concentrated, diluted with Et2O and the precipitate is collected.

後処理

  1. temperatureat reflux
  2. customExcess LiAlH4 is destroyed
  3. temperatureunder cooling
  4. filtrationAfter 30 min the mixture is filtered
  5. concentrationthe filtrate is concentrated
  6. additiondiluted with Et2O
  7. customthe precipitate is collected

出典と根拠

ORDレコード
ord-eb0c9a939d774358996ac3fe406ed8e9
出典データセット
uspto-grants-2013_07
特許番号
US08486968B2

反応ノート

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