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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

反応式

関与物質

役割名称HCID仕込み量
反応物Tris(propan-2-yl)silanethiolHCID 3435097—
反応物Sodium t-butoxideHCID 23676156—
反応物tert-Butyl 2-iodobenzyl(methyl)carbamateHCID 67018447—
触媒Bis[2-(diphenylphosphino)phenyl] etherHCID 4285986—
触媒Bis(dibenzylideneacetone)palladiumHCID 9811564—
溶媒TolueneHCID 1140—
生成物Methyl-(2-triisopropylsilanylsulfanyl-benzyl)-carbamic acid tert-butyl esterHCID 67018449387%

反応条件

温度160 °C

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

DOI10.6084/m9.figshare.5104873.v1
特許番号US07534791B2
出典データセットuspto-grants-2009_05
ORD IDord-b2416be841294e798e23e6aab34f8d16
出典メモuspto-grants-2009_05