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

HRID 1414270

반응식

HRID 1414270 반응식
[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

참가 물질

7

반응물 3

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

생성물 1

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

시약·촉매·용매 3

HCID 962Water용매2회HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-616492bc1aa24945ac82dba79019805e
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04001244

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