4-Hydroxybenzaldehyde → 3-(4-Formylphenoxy)propyltrimethoxysilane

HRID 236625

반응식

HRID 236625 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.CS(C)=O.[OH-].[Na+].Cl[CH2:17][CH2:18][CH2:19][Si:20]([O:25][CH3:26])([O:23][CH3:24])[O:21][CH3:22]>C1(C)C=CC=CC=1>[CH:6]([C:5]1[CH:8]=[CH:9][C:2]([O:1][CH2:17][CH2:18][CH2:19][Si:20]([O:25][CH3:26])([O:23][CH3:24])[O:21][CH3:22])=[CH:3][CH:4]=1)=[O:7]

참가 물질

6

반응물 4

HCID 1264-HydroxybenzaldehydeHCID 679Dimethyl SulfoxideHCID 14798Sodium Hydroxide2회HCID 624493-(Trimethoxysilyl)propyl chloride

생성물 1

HCID 1445353-(4-Formylphenoxy)propyltrimethoxysilane수율 85%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Using the general procedure described in the preceding Example 1, a reactor was charged with 62.2 g (0.55 mole) p-hydroxybenzaldehyde, 112 cc dimethylsulfoxide, 120 cc toluene and 43.2 g of a 50% aqueous sodium hydroxide solution containing 0.54 mole NaOH. All of the water present was removed by azeotropic distillation at a temperature of about 110° to 115° C. The reaction mixture was heated to the boiling point during the gradual addition of 109 g (0.55 mole) of 3-chloropropyl trimethoxysilane. The product, 3(p-formylphenoxy)propyl trimethoxysilane, was isolated by filtration and removal of the solvents from the recovered liquid phase under reduced pressure, followed by fractional distillation of the residue. The fraction boiling at 208° C. at a pressure of 3 mm of mercury was collected (85% yield, based on silane). The infrared and nuclear magnetic resonance spectra of the distillate confirm the proposed structure ##STR17## The vapor phase chromatogram of the product indicated a purity of greater than 98%.

후처리

  1. customAll of the water present was removed by azeotropic distillation at a temperature of about 110° to 115° C

출처 및 근거

ORD 기록
ord-19ce652934b74b5f963bda3501d19ea2
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04645844

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