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

HRID 1294139노트

반응식

HRID 1294139 반응식
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:20]=[C:19]([C:21](OC)=[O:22])[CH:18]=[CH:17][N:16]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.[O-]S([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:20]=[C:19]([CH2:21][OH:22])[CH:18]=[CH:17][N:16]=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-pyridylmethanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of methyl 2-(5-methyl-2-phenyl-4-oxazolyl)methoxy-4-pyridinecarboxylate (1.95 g) and tetrahydrofuran (20 mL) was added lithium aluminum hydride (0.228 g) under ice-cooling, and the mixture was stirred at room temperature for 30 min. Sodium sulfate 10 hydrate (1.93 g) was added to the mixture and the mixture was stirred at room temperature for 30 min. The insoluble materials were removed by filtration, and the filtrate was concentrated. The obtained crystals were recrystallized from ethyl acetate-hexane to give [2-(5-methyl-2-phenyl-4-oxazolylmethoxy)-4-pyridyl]methanol as colorless plate crystals (1.37 g, 77%). melting point: 100-101° C.

후처리

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 30 min
  3. customThe insoluble materials were removed by filtration
  4. concentrationthe filtrate was concentrated
  5. customThe obtained crystals were recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-24cfc1ea6b3f42f9bcd33ec9cbd0a40f
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07238716B2

반응 노트

불러오는 중…