Water → 3-(3,5-Dimethoxy-phenyl)-propan-1-OL

HRID 1434412ノート

反応式

HRID 1434412 の反応式
C([O:3][C:4](=O)[CH:5]=[CH:6][C:7]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[C:9]([O:15][CH3:16])[CH:8]=1)C.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[CH3:16][O:15][C:9]1[CH:8]=[C:7]([CH2:6][CH2:5][CH2:4][OH:3])[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=1

参加物

5

反応物 3

HCID 962WaterHCID 3346402HCID 3346402、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 113330533-(3,5-Dimethoxy-phenyl)-propan-1-OL

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Synthesized from 3-(3,5-dimethoxyphenyl)acrylic acid ethyl ester according to an analogous synthetic method to Example 22,ethyl 3-(3,5-dimethoxyphenyl)propionate (38.4 g) was added dropwise to a solution of lithium aluminum hydride (12.3 g) in tetrahydrofuran (200 ml) on an ice bath, and the solution was stirred for 15 minutes at room temperature. To the reaction solution were sequentially added water (12 ml), an aqueous solution of 5N sodium hydroxide (12 ml) and water (28 ml), the suspension was filtered, and then the solvent was evaporated in vacuo. The residue was purified by silica gel column chromatography (hexane-ethyl acetate system) to provide the title compound (24.3 g).

後処理

  1. filtrationan aqueous solution of 5N sodium hydroxide (12 ml) and water (28 ml), the suspension was filtered
  2. customthe solvent was evaporated in vacuo
  3. customThe residue was purified by silica gel column chromatography (hexane-ethyl acetate system)

出典と根拠

ORDレコード
ord-dedc4f391c3a4efe944b2c5dd37a5d13
出典データセット
uspto-grants-2009_11
特許番号
US07612114B2

反応ノート

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