Potassium Carbonate → 5-Bromo-3-methoxy-2-(2-trimethylsilanylethoxymethoxy)benzaldehyde

HRID 2234138

반응식

HRID 2234138 반응식
[Br:1][C:2]1[CH:3]=[C:4]([O:11][CH3:12])[C:5]([OH:10])=[C:6]([CH:9]=1)[CH:7]=[O:8].C(=O)([O-])[O-].[K+].[K+].[CH3:19][Si:20]([CH3:27])([CH3:26])[CH2:21][CH2:22][O:23][CH2:24]Cl>CN(C=O)C>[Br:1][C:2]1[CH:3]=[C:4]([O:11][CH3:12])[C:5]([O:10][CH2:24][O:23][CH2:22][CH2:21][Si:20]([CH3:27])([CH3:26])[CH3:19])=[C:6]([CH:9]=1)[CH:7]=[O:8]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2622385-Bromo-2-hydroxy-3-methoxybenzaldehydeHCID 27242712-Chloromethyl 2-(trimethylsilyl)ethyl ether

생성물 1

HCID 860709695-Bromo-3-methoxy-2-(2-trimethylsilanylethoxymethoxy)benzaldehyde

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

2 g of 5-Bromo-2-hydroxy-3-methoxy-benzaldehyde is dissolved in 200 ml of DMF and 4.78 g of potassium carbonate and 2.3 g of 2-trimethylsilyl-ethoxymethyl chloride are added. The reaction is stirred at RT for 18 h. The solvents are removed under reduced pressure, the residue is dissolved in ethyl acetate and washed with water. After drying over magnesium sulfate, filtration and evaporation, the product is purified by silica gel chromatography eluting with a gradient of ethyl acetate in heptane. Yield 1.8 g.

후처리

  1. customThe solvents are removed under reduced pressure
  2. dissolutionthe residue is dissolved in ethyl acetate
  3. washwashed with water
  4. dry with materialAfter drying over magnesium sulfate, filtration and evaporation
  5. customthe product is purified by silica gel chromatography
  6. washeluting with a gradient of ethyl acetate in heptane

출처 및 근거

ORD 기록
ord-35f46b2b9c7c4815a4434cf1b50f9ace
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709466B2

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