Sodium sulfate decahydrate → 2-(5-Methyl-2-phenyl-4-oxazolylmethoxy)-4-pyridylmethanol

HRID 349948노트

반응식

HRID 349948 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[O:12][C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:10][C:9]=1[CH2:19][O:20][C:21]1[CH:26]=[C:25]([C:27](OC)=[O:28])[CH:24]=[CH:23][N:22]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:7][C:8]1[O:12][C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:10][C:9]=1[CH2:19][O:20][C:21]1[CH:26]=[C:25]([CH2:27][OH:28])[CH:24]=[CH:23][N:22]=1

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 17861336Methyl 2-(5-methyl-2-phenyl-4-oxazolyl)methoxy-4-pyridinecarboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 178613752-(5-Methyl-2-phenyl-4-oxazolylmethoxy)-4-pyridylmethanol수율 77%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Lithium aluminium hydride (228 mg) was added to a solution of methyl 2-(5-methyl-2-phenyl-4-oxazolylmethoxy)-4-pyridinecarboxylate (1.95 g) in tetrahydrofuran (20 ml) at 0° C., which was stirred at room temperature for 30 minutes. Sodium sulfate decahydrate (1.93 g) was added to the reaction mixture, which was stirred at room temperature for 30 minutes. The precipitates were removed by filtration, the filtrate was concentrated. The resulting colorless crystals were collected by filtration to obtain 2-(5-methyl-2-phenyl-4-oxazolylmethoxy)-4-pyridylmethanol (1.37 g, yield 77%). This was recrystallized from ethyl acetate-hexane. Melting point: 100–101° C.

후처리

  1. stirringwas stirred at room temperature for 30 minutes
  2. customThe precipitates were removed by filtration
  3. concentrationthe filtrate was concentrated
  4. filtrationThe resulting colorless crystals were collected by filtration

출처 및 근거

ORD 기록
ord-1e87c65db03f4f78831acb664f1c0722
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179823B1

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