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Dimethyl Carbonate → 3,4-Dihydro-2-hydroxynaphthalenecarboxylic Acid, Methyl Ester

HRID 1421892
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HRID 1421892 반응식
[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][C:2]1=[O:11].C([N-]C(C)C)(C)C.[Li+].[C:20](=O)([O:23]C)[O:21][CH3:22]>O1CCCC1>[OH:11][C:2]1[CH2:3][CH2:4][C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[C:1]=1[C:20]([O:21][CH3:22])=[O:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

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HCID 12021Dimethyl CarbonateHCID 682662-TetraloneHCID 2724682Lithium diisopropylamide

생성물 1

HCID 546921643,4-Dihydro-2-hydroxynaphthalenecarboxylic Acid, Methyl Ester수율 100%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a stirred solution of 2-tetralone (25.0 g, 171 mmol) in dry tetrahydrofuran (250 ml) at 0° C. under argon was added lithium diisopropylamide (111 ml, 2M solution, 222 mmol). After stirring at 0° C. for 1 h, dimethyl carbonate was added (145 ml, 1710 mmol). After stirring at 0° C. for 0.5 h, the reaction mixture was warmed to room temperature, and then heated at reflux for 16 h. The mixture was then cooled to 0° C. and quenched with hydrochloric acid (1M, 450 ml). The resulting mixture was extracted with ethyl acetate (3×1000 ml) and the combined extracts were washed with brine (1000 ml) then dried (Na2SO4) and evaporated in vacuo to afford the title compound as a dark brown oil (36.3 g, 100%).

후처리

  1. stirringAfter stirring at 0° C. for 0.5 h
  2. temperaturethe reaction mixture was warmed to room temperature
  3. temperatureheated
  4. temperatureat reflux for 16 h
  5. temperatureThe mixture was then cooled to 0° C.
  6. customquenched with hydrochloric acid (1M, 450 ml)
  7. extractionThe resulting mixture was extracted with ethyl acetate (3×1000 ml)
  8. washthe combined extracts were washed with brine (1000 ml)
  9. dry with materialthen dried (Na2SO4)
  10. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-b9e614113f68465c89e5501eda65ed59
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06080752

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