참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | (2-Thienylmethyl)amine | HCID 34005 | — |
| 반응물 | 1,3-Bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane | HCID 75385 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-(2-Thienylmethyl)-2,2,6,6-tetra-methyl-1-oxa-4-aza-2,6-disilacyclohexane | HCID 23340295 | — |
반응 단계
To a solution containing 22.6 g. (0.2 mole) of 2-thenylamine, 44.4 g. (0.44 mole) of triethylamine and 50.0 g. of acetonitrile dried over molecular sieves there is added 46.2 g. (0.2 mole) of 1,3-bis-chloromethyl-1,1,3,3-tetramethyl-disiloxane. The resulting homogenized solution is allowed to stand for 3 days and then heated in a bath at 90° C. for 36 hours. After cooling the mixture is then equiliberated between toluene and water, the organic phase is then washed with two more portions of water and concentrated to give 61.5 g. of a crude oil. Vacuum distillation through a Vigreux column gives 4-(2-thienylmethyl)-2,2,6,6-tetra-methyl-1-oxa-4-aza-2,6-disilacyclohexane; b.p. 78° to 80° C. at 0.1 to 0.11 mm.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04224317 |
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| 출처 데이터셋 | uspto-grants-1980_09 |
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| ORD ID | ord-daa0191ef4ad4921942a85e01f0b9bb3 |
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| 출처 메모 | uspto-grants-1980_09 |
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