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

HRID 1109657

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HRID 1109657 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-4e7fd868d91048dbbb82401081de07de
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05321135

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