참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | Octanoyl chloride | HCID 8124 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1-Propanethiol, 3-(triethoxysilyl)- | HCID 84658 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | Octanethioic acid, S-(3-(triethoxysilyl)propyl) ester | HCID 12135713 | 99.2% |
반응 단계
Into a 12-liter, three-necked round bottom flask equipped with mechanical stirrer, addition funnel, thermocouple, heating mantle, N2 inlet, and temperature controller were charged 3-mercaptopropyltriethoxysilane (1,021 grams, 3.73 moles purchase as SILQUEST® A-1891 silane from Momentive Performance Materials, Inc.), triethylamine (433 grams), and hexane (3,000 ml). The solution was cooled in an ice bath, and octanoyl chloride (693 grams, 4.25 moles) were added over a two hour period via the addition funnel. After addition of the acid chloride was complete, the mixture was filtered two times, first through a 0.1 μm filter and then through a 0.01 μm filter, using a pressure filter, to remove the salt. The solvent was removed under vacuum. The remaining yellow liquid was vacuum distilled to yield 1,349 grams of octanoylthiopropyltriethoxysilane as a clear, very light yellow liquid. The yield was 87 percent.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09447262B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-cc4ab92194bd493f9ad2faa2b80e1bab |
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| 출처 메모 | uspto-grants-2016_09 |
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