Triethylamine → 2-(2-Methoxypyridin-3-yl)acetaldehyde

HRID 1837705노트

반응식

HRID 1837705 반응식
[CH3:1][O:2][C:3]1[C:8]([CH2:9][CH2:10][OH:11])=[CH:7][CH:6]=[CH:5][N:4]=1.C(N(CC)CC)C.C(=O)(O)[O-].[Na+]>CS(C)=O>[CH3:1][O:2][C:3]1[C:8]([CH2:9][CH:10]=[O:11])=[CH:7][CH:6]=[CH:5][N:4]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 140623082-(2-Methoxy-3-pyridinyl)ethanol

생성물 1

HCID 226786312-(2-Methoxypyridin-3-yl)acetaldehyde수율 16.9%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

실험 절차

A solution of 2.7 g of pyridine-sulfur trioxide complex dissolved in DMSO was added dropwise at 20° C. or less to a solution of 1.2 g of 2-(2-methoxy-3-pyridyl)ethanol and 4.8 ml of triethylamine dissolved in DMSO. After stirring for 0.5 hour, a cooled sodium bicarbonate was added thereto, and the mixture was extracted with ethyl acetate. After drying over sodium sulfate, the solvent was evaporated. The residue was purified by silica gel chromatography (hexane:ethyl acetate=4:1), to give 200 mg of a yellow oil.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialAfter drying over sodium sulfate
  3. customthe solvent was evaporated
  4. customThe residue was purified by silica gel chromatography (hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-c291d7359dc945199dd859cba9edd73b
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06784192B2

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