참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Piperazine | HCID 4837 | — |
| 반응물 | Silane | HCID 23953 | — |
| 반응물 | Piperazine, hydrochloride (1:?) | HCID 82044 | — |
| 반응물 | Silane, (chloromethyl)triethoxy- | HCID 84858 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | N-triethoxysilyl-methylpiperazine | HCID 67062407 | — |
반응 단계
905.3 g (10.5 mol) of piperazine and 945 ml of xylene (anhydrous) as solvent are charged to a 4 liter 4-neck flask and subsequently innertized with nitrogen. The batch is heated to a temperature of 100° C., in the course of which the piperazine dissolves completely. Added dropwise at this temperature are 446.3 g (2.1 mol) of chloromethyltriethoxysilane, over the course of 1 h with thorough stirring. Following the addition of about ⅓ of the amount of silane, piperazine hydrochloride is precipitated as a salt, but the suspension remains readily stirrable until the end of the reaction. After the end of the addition, stirring is continued for a further 15 min. Subsequently the reaction mixture is heated to 110° C. and the precipitated salt is filtered off on a preheated filter.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07906179B2 |
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| 출처 데이터셋 | uspto-grants-2011_03 |
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| ORD ID | ord-045ff6c78d274fb1a672d1d1591d8ae4 |
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| 출처 메모 | uspto-grants-2011_03 |
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