참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | 3-(Diethylamino)phenol | HCID 7062 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 3-(Trimethoxysilyl)propyl chloride | HCID 62449 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3(m-diethylaminophenoxy)propyl Trimethoxysilane | HCID 13879171 | — |
반응 단계
Using the general procedure described in the preceding Example 1, a reactor was charged with 90.75 g (0.55 mole) m-diethylaminophenol, 112 cc dimethylsulfoxide, 120 cc toluene and 43.28 g of a 50% aqueous sodium hydroxide solution. All of the water present in the reactor was removed by azeotropic distillation. The reaction mixture was allowed to cool to 80° C., at which time 109 g (0.55 mole) of chloropropyl trimethoxysilane were gradually added over a period of 2 hours. The temperature of the reaction mixture increased to 88° C. during the addition. Following completion of the addition, external heating was applied to maintain the temperature of the reaction mixture at 80° C. for 16 hours. The reaction mixture was then allowed to cool and was filtered. The liquid phase was recovered and evaporated under a pressure of 5 mm of mercury to remove the toluene and dimethylsulfoxide. The pressure inside the reactor was reduced to 2 mm and the product, 3(m-diethylaminophenoxy)propyl trimethoxysilane, distilled at a temperature of 185°-187° C. Analysis by vapor phase chromatography demonstrated that the product was 97% pure.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04645844 |
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| 출처 데이터셋 | uspto-grants-1987_02 |
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| ORD ID | ord-6dde650ddd7e42268a8fc88a111cd5fd |
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| 출처 메모 | uspto-grants-1987_02 |
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