Water → 4-Aminomethylbenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether

HRID 483714

반응식

HRID 483714 반응식
[CH3:1][C:2]1([CH3:24])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([O:14][CH2:15][C:16]3[CH:21]=[CH:20][C:19]([C:22]#[N:23])=[CH:18][CH:17]=3)[CH:5]=[CH:4][C:3]1=2.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.S([O-])([O-])(=O)=O.[Na+].[Na+]>CCOCC>[CH3:1][C:2]1([CH3:24])[CH2:11][CH2:10][C:9]([CH3:12])([CH3:13])[C:8]2[CH:7]=[C:6]([O:14][CH2:15][C:16]3[CH:21]=[CH:20][C:19]([CH2:22][NH2:23])=[CH:18][CH:17]=3)[CH:5]=[CH:4][C:3]1=2

참가 물질

6

반응물 4

HCID 962WaterHCID 24436Sodium SulfateHCID 148505774-Cyanobenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl etherHCID 21226445Aluminium lithium hydride

생성물 1

HCID 148505814-Aminomethylbenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A suspension of 3 g (9.4 mmol) of 4-cyanobenzyl 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyl ether in 60 ml of ether was added dropwise under nitrogen to a suspension of 1 g (26 mmol) of lithium aluminum hydride in 50 ml of dry ether at 25° C. The mixture was then stirred under reflux for 3 h, cooled and hydrolyzed cautiously with water and sodium sulfate solution. The mixture was extracted three times with ether, and the combined ether extracts were washed with water, dried over Na2SO4 and concentrated. 3 g of the title compound of melting point 77°-79° C. remained.

후처리

  1. temperatureunder reflux for 3 h
  2. temperaturecooled
  3. extractionThe mixture was extracted three times with ether
  4. washthe combined ether extracts were washed with water
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2359a7ce6aa7487d9fc7aeca30dfb26f
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05225601

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