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Thionyl Chloride → 2-Chloromethyl-6-(5-methyl-2-phenyl-4-oxazolylmethoxy)pyridine

HRID 1294142
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HRID 1294142 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[N:20]=[C:19]([C:21](OC)=O)[CH:18]=[CH:17][CH: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+].S(Cl)([Cl:50])=O>O1CCCC1>[Cl:50][CH2:21][C:19]1[CH:18]=[CH:17][CH:16]=[C:15]([O:14][CH2:13][C:3]2[N:4]=[C:5]([C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=3)[O:6][C:2]=2[CH3:1])[N:20]=1
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참가 물질

6

반응물 4

HCID 24386Thionyl ChlorideHCID 62649Sodium sulfate decahydrateHCID 17861391Methyl 6-(5-methyl-2-phenyl-4-oxazolyl)methoxy-2-pyridinecarboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 178613022-Chloromethyl-6-(5-methyl-2-phenyl-4-oxazolylmethoxy)pyridine

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

To a mixture of methyl 6-(5-methyl-2-phenyl-4-oxazolyl)methoxy-2-pyridinecarboxylate (6.49 g) and tetrahydrofuran (60 mL) was added lithium aluminum hydride (0.759 g) under ice-cooling, and the mixture was stirred at room temperature for 30 min. To the mixture was added sodium sulfate 10 hydrate (6.44 g) and further stirred at room temperature for 30 min. The insoluble materials were removed by filtration, and the filtrate was concentrated to give crystals. The obtained crystals were added to thionyl chloride (20 mL) under ice-cooling, and the mixture was stirred at room temperature for 1 hr. The reaction mixture was concentrated, saturated aqueous sodium hydrogencarbonate was added to the residue and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated. The obtained residue was subjected to silica gel column chromatography to give crystals of 2-chloromethyl-6-(5-methyl-2-phenyl-4-oxazolylmethoxy)pyridine from a fraction eluted with ethyl acetate-hexane (1:3, v/v). Recrystallization from ethyl acetate-hexane gave colorless plate crystals (2.74 g, 44%). melting point: 85-86° C.

후처리

  1. temperaturecooling
  2. stirringfurther stirred at room temperature for 30 min
  3. customThe insoluble materials were removed by filtration
  4. concentrationthe filtrate was concentrated
  5. customto give crystals
  6. temperaturecooling
  7. stirringthe mixture was stirred at room temperature for 1 hr
  8. concentrationThe reaction mixture was concentrated
  9. additionsaturated aqueous sodium hydrogencarbonate was added to the residue
  10. extractionthe mixture was extracted with ethyl acetate
  11. washThe organic layer was washed with saturated brine
  12. dry with materialdried over anhydrous magnesium sulfate
  13. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8a8317de88994b77a68b9854d29b03b8
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07238716B2

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