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Sodium sulfate decahydrate → 3-Methyl-3-(2-methylquinolin-8-yl)butan-1-ol

HRID 339039
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HRID 339039 반응식
[CH3:1][C:2]([C:10]1[CH:11]=[CH:12][CH:13]=[C:14]2[C:19]=1[N:18]=[C:17]([CH3:20])[CH:16]=[CH:15]2)([CH3:9])[CH2:3][C:4](OCC)=[O:5].[H-].[H-].[H-].[H-].[Li+].[Al+3].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH3:9][C:2]([C:10]1[CH:11]=[CH:12][CH:13]=[C:14]2[C:19]=1[N:18]=[C:17]([CH3:20])[CH:16]=[CH:15]2)([CH3:1])[CH2:3][CH2:4][OH:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 70984548Ethyl 3-methyl-3-(2-methylquinolin-8-yl)butanoate

생성물 1

HCID 709836813-Methyl-3-(2-methylquinolin-8-yl)butan-1-ol수율 100.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

To a solution of ethyl 3-methyl-3-(2-methylquinolin-8-yl)butanoate (0.66 g, 2.43 mmol) in THF (3 mL) was added 1.0 N LAH (3.65 mL, 3.65 mmol) in THF at 0° C. and stirred at 0° C. for 3 hours. Sodium sulfate decahydrate (2.0 g) was added and stirred at ambient temperature for 30 minutes. The solid was removed by filtration and washed with ethyl acetate (30 mL). The filtrate was concentrated under reduced pressure to give 3-methyl-3-(2-methylquinolin-8-yl)butan-1-ol (0.56 g, 100%) as a solid.

후처리

  1. stirringstirred at ambient temperature for 30 minutes
  2. customThe solid was removed by filtration
  3. washwashed with ethyl acetate (30 mL)
  4. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-23c707aa913b48f2a10d83ad28b916af
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08889704B2

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