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HRID 493092作成日:2026年10月26日
Tris(propan-2-yl)silanethiol → Methyl-(2-triisopropylsilanylsulfanyl-benzyl)-carbamic acid tert-butyl ester
https://huagongshe.com/reaction/493092
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tris(propan-2-yl)silanethiol | HCID 3435097 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 反応物 | tert-Butyl 2-iodobenzyl(methyl)carbamate | HCID 67018447 | — |
| 触媒 | Bis[2-(diphenylphosphino)phenyl] ether | HCID 4285986 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl-(2-triisopropylsilanylsulfanyl-benzyl)-carbamic acid tert-butyl ester | HCID 67018449 | 387% |
反応手順
(2-Iodo-benzyl)-methyl-carbamic acid tert-butyl ester (3.0 g, 8.64 mmol), tris(dibenzylideneacetone)dipalladium (0) (79 mg, 0.086 mmol), bis(2-diphenylphosphinophenyl)ether (93 mg, 0.17 mmol), sodium tert-butoxide (1.10 g, 11.2 mmol), triisopropylsilanethiol (1.73 g, 9.07 mmol) and dry toluene (15 mL) are all placed in an Emrys Optimizer EXP 20 mL microwave reactor tube. The reaction vessel is sealed and subjected to microwave heating at 160° C. for 15 minutes. Upon cooling the mixture is poured onto a plug of silica and the product is eluted with ethyl acetate-heptane (1:4). This procedure is repeated an additional 3 times to furnish a total of 13.7 g (97%) of the title compound as an oil which is used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07534791B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-b2416be841294e798e23e6aab34f8d16 |
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| 出典メモ | uspto-grants-2009_05 |
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