4-Hydroxybenzaldehyde → 4-Trimethylsilanylmethoxybenzaldehyde

HRID 899016

반응식

HRID 899016 반응식
Cl[CH2:2][Si:3]([CH3:6])([CH3:5])[CH3:4].[OH:7][C:8]1[CH:15]=[CH:14][C:11]([CH:12]=[O:13])=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:4][Si:3]([CH2:2][O:7][C:8]1[CH:15]=[CH:14][C:11]([CH:12]=[O:13])=[CH:10][CH:9]=1)([CH3:6])[CH3:5]

참가 물질

5

반응물 3

HCID 1264-HydroxybenzaldehydeHCID 11430Potassium CarbonateHCID 75361Silane, (chloromethyl)trimethyl-

생성물 1

HCID 565289644-Trimethylsilanylmethoxybenzaldehyde수율 84%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

Chloromethyltrimethylsilane (110.5 g, 0.9 mol) is added dropwise over 30 minutes to a mixture of para-hydroxybenzaldehyde (110 g, 0.82 mol) and potassium carbonate (124.5 g, 0.9 mol) in 1 L of dry DMF maintained at 80° C., and while sparging with nitrogen. The mixture is left at 90° C. for 4 hours. The reaction mixture is filtered and the solvent is removed from the filtrate by distillation under vacuum. The final traces of DMF are removed via a stage at 60° C. under a vacuum of 2 mmHg. 142.4 g (yield: 84%) of 4-trimethylsilanylmethoxybenzaldehyde are obtained in the form of an orange-yellow oil, which is used without further purification in the next step.

후처리

  1. customwhile sparging with nitrogen
  2. filtrationThe reaction mixture is filtered
  3. customthe solvent is removed from the filtrate by distillation under vacuum
  4. customThe final traces of DMF are removed via a stage at 60° C. under a vacuum of 2 mmHg

출처 및 근거

ORD 기록
ord-dfab117446f04b698ae0f92944dbd878
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07354571B2

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