Water → 4-Hydroxymethyl-2-(3,4,5-trimethoxyphenyl)pyridine

HRID 395416노트

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HRID 395416 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:13]2[CH:14]=[C:15]([CH:21]=[CH:22][N:23]=2)[C:16](OCC)=[O:17])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[OH:17][CH2:16][C:15]1[CH:21]=[CH:22][N:23]=[C:13]([C:5]2[CH:6]=[C:7]([O:11][CH3:12])[C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[CH:14]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24436Sodium SulfateHCID 16125879Ethyl 2-(3,4,5-trimethoxyphenyl)pyridine-4-carboxylateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 161259364-Hydroxymethyl-2-(3,4,5-trimethoxyphenyl)pyridine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

Ethyl 2-(3,4,5-trimethoxyphenyl)isonicotinate (24.57 g) was dissolved in dry THF (200 mL), and to the solution lithium aluminum hydride (2.94 g) was added at 0° C. under an argon atmosphere. The mixture was stirred at 0° C. for 1 hour as it is. A small amount of water and then sodium sulfate were added to the reaction mixture, and the reaction mixture was filtered through celite. The filtrate was evaporated, and the reultant crude crystals were recrystalized from ethyl acetate-hexane to give the title compound.

후처리

  1. filtrationthe reaction mixture was filtered through celite
  2. customThe filtrate was evaporated
  3. customthe reultant crude crystals were recrystalized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-64bb0663e2c0480593b178f712623a2f
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06605620B1

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