関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (2-Thienylmethyl)amine | HCID 34005 | — |
| 反応物 | 1,3-Bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane | HCID 75385 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(2-Thienylmethyl)-2,2,6,6-tetra-methyl-1-oxa-4-aza-2,6-disilacyclohexane | HCID 23340295 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04224317 |
|---|
| 出典データセット | uspto-grants-1980_09 |
|---|
| ORD ID | ord-daa0191ef4ad4921942a85e01f0b9bb3 |
|---|
| 出典メモ | uspto-grants-1980_09 |
|---|