Water → 2-Naphthalenemethanol, 5,6-dihydro-7-(1H-imidazol-1-yl)-

HRID 1980549노트

반응식

HRID 1980549 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[N:7]1([C:12]2[CH2:13][CH2:14][C:15]3[C:20]([CH:21]=2)=[CH:19][C:18]([C:22](OCC)=[O:23])=[CH:17][CH:16]=3)[CH:11]=[CH:10][N:9]=[CH:8]1.O>C1COCC1>[N:7]1([C:12]2[CH2:13][CH2:14][C:15]3[C:20]([CH:21]=2)=[CH:19][C:18]([CH2:22][OH:23])=[CH:17][CH:16]=3)[CH:11]=[CH:10][N:9]=[CH:8]1

참가 물질

5

반응물 3

HCID 962WaterHCID 30215662-Naphthalenecarboxylic acid, 5,6-dihydro-7-(1H-imidazol-1-yl)-, ethyl esterHCID 21226445Aluminium lithium hydride

생성물 1

HCID 30215682-Naphthalenemethanol, 5,6-dihydro-7-(1H-imidazol-1-yl)-수율 84.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of LiAlH4 (202 mg) in dry THF (2.4 ml) a solution of 1,2-dihydro-3-(1-imidazolyl)-6-ethoxycarbonyl-naphthalene (2.8 g) in dry THF (22 ml) was added dropwise at 0° C. under nitrogen atmosphere. The reaction mixture was refluxed for 1 day and then stirred overnight at room temperature. H2O (40 ml) was added and the precipitate formed filtered off. The filtrate was concentrated, extracted with CHCl3, dried (Na2SO4) and evaporated under vacuum to give 1,2-dihydro-3-(1-imidazolyl)-6-hydroxymethyl-naphthalene (2 g).

후처리

  1. additionwas added dropwise at 0° C. under nitrogen atmosphere
  2. temperatureThe reaction mixture was refluxed for 1 day
  3. customthe precipitate formed
  4. filtrationfiltered off
  5. concentrationThe filtrate was concentrated
  6. extractionextracted with CHCl3
  7. dry with materialdried (Na2SO4)
  8. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-6d7e02ef6c954b65ac213386db35bfc9
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04510149

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