Water → (4'-Methoxy[1,1'-biphenyl]-4-yl)methanol

HRID 1072703

反応式

HRID 1072703 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:18]=[CH:17][C:12]([C:13](OC)=[O:14])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[CH:18]=[CH:17][C:12]([CH2:13][OH:14])=[CH:11][CH:10]=2)=[CH:7][CH:8]=1

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 1393415Methyl 4'-methoxy(1,1'-biphenyl)-4-carboxylateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 1051637(4'-Methoxy[1,1'-biphenyl]-4-yl)methanol収率 45.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

Methyl 4-(4′-methoxyphenyl)benzoate (3.0 g, 12.3 mmol) was added in portions to a suspension of lithium aluminum hydride (0.94 g, 25.0 mmol) in tetrahydrofuran (40 ml) at room temperature for 20 minutes with stirring. The reaction solution was refluxed for 2 hours under heating and cooled to 0° C. To the residue was added water (1 ml) and 1 N aqueous sodium hydroxide (3 ml), the insoluble matter was filtered out and the filtrate was concentrated under reduced pressure. The object compound (1.2 g) was obtained from the residue as colorless crystals.

後処理

  1. temperatureThe reaction solution was refluxed for 2 hours
  2. temperatureunder heating
  3. filtrationthe insoluble matter was filtered out
  4. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-5d216088228f4668997d23a1dc2d4284
出典データセット
uspto-grants-2005_06
特許番号
US06911468B2

関連ノート

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