Sodium sulfate decahydrate → 3-(3,4,5-Trimethoxyphenyl)Propan-1-Ol

HRID 1109657ノート

反応式

HRID 1109657 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:13][CH2:14][C:15](OC)=[O:16])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:12][O:11][C:7]1[CH:6]=[C:5]([CH2:13][CH2:14][CH2:15][OH:16])[CH:4]=[C:3]([O:2][CH3:1])[C:8]=1[O:9][CH3:10]

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 2797678Methyl 3-(3,4,5-trimethoxyphenyl)propanoateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 64288433-(3,4,5-Trimethoxyphenyl)Propan-1-Ol収率 97.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of methyl 3-(3,4,5-trimethoxyphenyl)propanoate (11.03 g, 0.043 mol) in tetrahydrofuran (20 ml) was added dropwise to a suspension of lithium aluminum hydride (1.6 g, 0.042 mol) in 20 ml of tetrahydrofuran, said suspension having been cooled to 0° C., followed by stirring at room temperature for 19 hours. After the addition of sodium sulfate decahydrate, the resulting mixture was stirred further at room temperature for one hour. Insoluble matter was removed by filtration and the filtrate was concentrated, whereby 9.5 g of the title compound were obtained as colorless oil (yield: 96.8%).

後処理

  1. stirringthe resulting mixture was stirred further at room temperature for one hour
  2. customInsoluble matter was removed by filtration
  3. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-4e7fd868d91048dbbb82401081de07de
出典データセット
uspto-grants-1994_06
特許番号
US05321135

反応ノート

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