Methanol → 2-Phenylbutane-1,2-diamine

HRID 2227452ノート

反応式

HRID 2227452 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[NH2:7][C:8]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)([CH2:11][CH3:12])[C:9]#[N:10].CO>CCOCC.C(Cl)Cl>[C:13]1([C:8]([NH2:7])([CH2:11][CH3:12])[CH2:9][NH2:10])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

6

反応物 3

HCID 887MethanolHCID 167944572-Amino-2-phenylbutanenitrileHCID 21226445Aluminium lithium hydride

生成物 1

HCID 211492-Phenylbutane-1,2-diamine収率 81%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

To a stirred suspension of lithium aluminum hydride (LAH, 7.0 g) in 250 mL of ether is added dropwise a solution of the compound of step 1(10.0 g) in 10 mL of ether at −70° C. The reaction mixture is stirred at −60° C. to −70° C. until TLC (10% MeOH in CH2Cl2) shows the disappearance of the starting material. The excess LAH is destroyed by cautious addition of a saturated aqueous Na2SO4 solution. The resulting mixture is filtered and solid is washed with EtOAc. The filtrate is dried over Na2SO4 and concentrated under vacuum to give 8.3 g of the title compound as clear oil.

後処理

  1. customThe excess LAH is destroyed by cautious addition of a saturated aqueous Na2SO4 solution
  2. filtrationThe resulting mixture is filtered
  3. washsolid is washed with EtOAc
  4. dry with materialThe filtrate is dried over Na2SO4
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-d6ee337e164742759ca44d393570b26f
出典データセット
uspto-grants-2002_07
特許番号
US06413982B1

反応ノート

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