Water → (7-Methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)methanol

HRID 2165157노트

반응식

HRID 2165157 반응식
C([O:3][C:4]([CH:6]1[CH2:15][CH2:14][C:13]2[C:8](=[CH:9][C:10]([O:16][CH3:17])=[CH:11][CH:12]=2)[CH2:7]1)=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1.C(OCC)C>[CH3:17][O:16][C:10]1[CH:9]=[C:8]2[C:13]([CH2:14][CH2:15][CH:6]([CH2:4][OH:3])[CH2:7]2)=[CH:12][CH:11]=1

참가 물질

7

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 54368774Ethyl 7-methoxy-1,2,3,4-tetrahydro-2-naphthalenecarboxylate

생성물 1

HCID 10797825(7-Methoxy-1,2,3,4-tetrahydronaphthalen-2-yl)methanol

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 23.43 g (100 mmol) of 7-methoxy-1,2,3,4-tetrahydro-naphthalene-2-carboxylic acid ethyl ester in 160 ml of absolute tetrahydrofuran is added dropwise, over a period of 30 minutes, while stirring at room temperature, to a suspension of 3.79 g (100 mmol) of lithium aluminium hydride in 160 ml of absolute diethyl ether. After stirring at room temperature for 1 hour, 3.8 ml of water, 3.8 ml of sodium hydroxide solution (15%) and 11.4 ml of water are added to the reaction mixture. The resulting precipitate is filtered off with suction and the filtrate is concentrated to dryness by evaporation in vacuo. The oily residue is dissolved in diethyl ether, washed with water, dried with sodium sulphate and concentrated to dryness by evaporation. 7-methoxy-1,2,3,4-tetrahydro-naphthalene-2-methanol is obtained in the form of a yellow oil.

후처리

  1. filtrationThe resulting precipitate is filtered off with suction
  2. concentrationthe filtrate is concentrated to dryness by evaporation in vacuo
  3. dissolutionThe oily residue is dissolved in diethyl ether
  4. washwashed with water
  5. dry with materialdried with sodium sulphate
  6. concentrationconcentrated to dryness by evaporation

출처 및 근거

ORD 기록
ord-f9243f24a0c54d56a6157720f598b2b9
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04939160

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