Sodium Hydroxide → 2-(3-(Benzyloxy)-4-methoxyphenyl)ethanamine

HRID 1414270

反応式

HRID 1414270 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([O:14][C:15]1[CH:16]=[C:17]([CH:23]=[CH:24][C:25]=1[O:26][CH3:27])[CH:18]=[CH:19][N+:20]([O-])=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[OH-].[Na+]>O.O1CCCC1.C(OCC)C>[CH2:7]([O:14][C:15]1[CH:16]=[C:17]([CH:23]=[CH:24][C:25]=1[O:26][CH3:27])[CH2:18][CH2:19][NH2:20])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

参加物

7

反応物 3

HCID 14798Sodium HydroxideHCID 2332022-Benzyloxy-1-methoxy-4-(2-nitrovinyl)benzeneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 27941762-(3-(Benzyloxy)-4-methoxyphenyl)ethanamine

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a suspension of 20 parts of lithium aluminum hydride in 444 parts of tetrahydrofuran and 177 parts of ethyl ether is added portionwise, over a 1 hour period, a warm solution of 56 parts of 3-benzyloxy-4-methoxy-β-nitrostyrene in 267 parts of tetrahydrofuran. The reaction mixture is refluxed for an additional 2 hours, then is cooled in ice and decomposed by adding 40 parts of water in 71 parts of tetrahydrofuran, followed by 40 parts by volume of a 25% by weight aqueous sodium hydroxide solution, followed by 40 parts of water. The salts are removed by filtration and the filtrate is dried over anhydrous calcium sulfate and stripped of solvent under reduced pressure to afford, as an oil, 3-benzyloxy-4-methoxyphenethylamine.

後処理

  1. additionis added portionwise, over a 1 hour period
  2. temperatureThe reaction mixture is refluxed for an additional 2 hours
  3. temperatureis cooled in ice
  4. customThe salts are removed by filtration
  5. dry with materialthe filtrate is dried over anhydrous calcium sulfate

出典と根拠

ORDレコード
ord-616492bc1aa24945ac82dba79019805e
出典データセット
uspto-grants-1977_01
特許番号
US04001244

関連ノート

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