Aluminium lithium hydride → 2-(6-Chloropyridin-3-yl)ethan-1-amine

HRID 76147ノート

反応式

HRID 76147 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][C:9]([NH2:11])=O)=[CH:4][CH:3]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][CH2:9][NH2:11])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydrideHCID 532788782-(6-Chloropyridin-3-YL)acetamide

生成物 1

HCID 204834902-(6-Chloropyridin-3-yl)ethan-1-amine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 2.00 g (11.7 mmol) 2-(6-chloropyridin-3-yl)-acetamide in 50 mL THF at 0° C. are added 12.9 ml LAH (c=1 mol/l in THF) by a dropping funnel. Cooling is removed and the reaction mixture is stirred for 1 h at r.t., then 8 ml LAH (c=1 mol/l in THF) are added and the reaction mixture is stirred at r.t. over night. The reaction is carefully quenched by the addition of 2 ml of an aq. NaHCO3 solution (10%). The mixture is filtrated and the solvent is removed under reduced pressure. The crude product is used without further purification.

後処理

  1. temperatureCooling
  2. customis removed
  3. addition8 ml LAH (c=1 mol/l in THF) are added
  4. stirringthe reaction mixture is stirred at r.t. over night
  5. customThe reaction is carefully quenched by the addition of 2 ml of an aq. NaHCO3 solution (10%)
  6. filtrationThe mixture is filtrated
  7. customthe solvent is removed under reduced pressure
  8. customThe crude product is used without further purification

出典と根拠

ORDレコード
ord-6fa8e2e68557410f80bfcc1187747a94
出典データセット
uspto-grants-2014_09
特許番号
US08835472B2

反応ノート

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