3-Ethoxy-4-methoxybenzonitrile → (3-Ethoxy-4-methoxyphenyl)methanamine

HRID 1934726

反応式

HRID 1934726 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([O:9][C:10]1[CH:11]=[C:12]([CH:15]=[CH:16][C:17]=1[O:18][CH3:19])[C:13]#[N:14])[CH3:8].C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>O1CCCC1.C(OCC)(=O)C>[CH2:7]([O:9][C:10]1[CH:11]=[C:12]([CH:15]=[CH:16][C:17]=1[O:18][CH3:19])[CH2:13][NH2:14])[CH3:8]

参加物

6

反応物 3

HCID 39347693-Ethoxy-4-methoxybenzonitrileHCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 6486613(3-Ethoxy-4-methoxyphenyl)methanamine収率 100.6%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

To a suspension of lithium aluminum hydride (1.17 g) in anhydrous tetrahydrofuran (15 mL) was added a solution of 3-ethoxy-4-methoxybenzonitrile (2.73 g) in tetrahydrofuran (15 mL). The mixture was stirred for an hour under water cooling and then for an hour at ambient temperature. Potassium sodium (+)-tartrate aqueous solution was added to the mixture under ice-water cooling. The mixture was diluted with ethyl acetate and the insolubles were filtered off. After evaporation of the filtrate, ethyl acetate was added. The solution was dried over magnesium sulfate and evaporated in vacuo to give 3-ethoxy-4-methoxybenzylamine as yellow oil (2.81 g).

後処理

  1. waitfor an hour at ambient temperature
  2. filtrationthe insolubles were filtered off
  3. customAfter evaporation of the filtrate, ethyl acetate
  4. additionwas added
  5. dry with materialThe solution was dried over magnesium sulfate
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-bd12492f2f9442299de08c06bcf8f529
出典データセット
uspto-grants-2002_05
特許番号
US06384080B1

関連ノート

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