Diethyl Ether → (4'-Methyl(1,1'-biphenyl)-4-yl)methanol

HRID 1903713노트

반응식

HRID 1903713 반응식
C[C:2]1([C:14]([O:16]C)=O)[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:4][CH2:3]1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+].[O-]S([O-])(=O)=O.[Na+].[Na+].[CH3:33]COCC>C1COCC1>[CH3:33][C:11]1[CH:10]=[CH:9][C:8]([C:5]2[CH:4]=[CH:3][C:2]([CH2:14][OH:16])=[CH:7][CH:6]=2)=[CH:13][CH:12]=1

참가 물질

7

반응물 5

HCID 3283Diethyl Ether2회HCID 14798Sodium HydroxideHCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydrideHCID 86738513Methyl 4-methyl[1,1-biphenyl]-4-carboxylate

생성물 1

HCID 1394290(4'-Methyl(1,1'-biphenyl)-4-yl)methanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

4-Methyl-(1,1'-biphenyl)-4-carboxylic acid, methyl ester (1.43 g) in ether (25 ml) and THF (25 ml) was added over 5 min to LiAlH4 (420 mg) in ether (25 ml). The mixture was stirred at room temperature for 1 h and then cooled in ice. Aqueous NaOH (1 M, 2.1 ml) was added and after stirring (15 min) excess anhydrous Na2SO4 was added. The mixture was filtered and the filtrate evaporated to give a solid. Crystallisation from cyclohexane-methanol gave the title compound (1.04 g) m.p. 128°-31°.

후처리

  1. temperaturecooled in ice
  2. additionwas added
  3. filtrationThe mixture was filtered
  4. customthe filtrate evaporated
  5. customto give a solid
  6. customCrystallisation from cyclohexane-methanol

출처 및 근거

ORD 기록
ord-545c32b37da643fda45c8eda0236a6b0
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04438112

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