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

HRID 1934726

반응식

HRID 1934726 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 6486613(3-Ethoxy-4-methoxyphenyl)methanamine수율 100.6%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-bd12492f2f9442299de08c06bcf8f529
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06384080B1

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