関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Vinylboronic acid | HCID 4683185 | — |
| 反応物 | (5-Chloro-2-nitro-4-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester | HCID 69489376 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (2-Nitro-4-trifluoromethyl-5-vinyl-phenyl)-carbamic acid tert-butyl ester | HCID 69486631 | 37% |
反応手順
A suspension of (5-chloro-2-nitro-4-trifluoromethyl-phenyl)-carbamic acid tert-butyl ester (Example A1) (6.8 g, 20 mmol), vinyl boronic acid [CAS-No. 4363-34-2] {Bull. Soc. Chim. Fr. 1966, (8), 2557-64} (4.312 g, 60 mmol) and K2CO3 (8.29 g, 60 mmol) in water (10 mL) and dioxane (50 mL) was purged by Ar-stream at 23° C. for 10 min, then tetrakis(triphenylphosphine)palladium(0) (693 mg, 0.6 mmol) was added and the mixture was heated to 100° C. for 20 h, filtered, evaporated and purified by column chromatography on silica gel (hexane/ethyl acetate 9:1) to yield a light yellow solid (2.476 g, 37%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06949542B2 |
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| 出典データセット | uspto-grants-2005_09 |
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| ORD ID | ord-71f366f258ee48e0874c000bee847ff0 |
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| 出典メモ | uspto-grants-2005_09 |
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