関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Benzenesulfonic Acid | HCID 7371 | — |
| 反応物 | Chlorodicyclohexylphosphine | HCID 2734135 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(Dicyclohexylphosphino)benzenesulfonic acid | HCID 19009137 | — |
反応手順
n-Butyllithium (manufactured by Kanto Chemical Co., Inc., 1.65 M hexane solution, 5.1 ml, 8.4 mmol) was added to a tetrahydrofuran (THF) solution (20 ml) of benzenesulfonic acid (manufactured by Tokyo Chemical Industry Co., Ltd., 0.66 g, 4.2 mmol) at 0° C. under argon atmosphere and the mixture was stirred for 2.5 hours at room temperature. After cooling the reaction container to −78° C., chlorodicyclohexylphosphine (manufactured by Sigma-Aldrich, 0.89 mg, 3.8 mmol) was added thereto at −78° C. and stirred for 24 hours at room temperature. After ceasing the reaction with trifluoroacetic acid (manufactured by Tokyo Chemical Industry Co., Ltd., 0.50 M THF solution, 8.4 ml, 4.2 mmol), the precipitate formed was collected by filtration and dried under reduced pressure to obtain 2-(dicyclohexylphosphino)benzenesulfonic acid (compound 1a). The yield was 0.66 g (85%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08889805B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-72a42cbe9b3a44939e5eac43ee92e958 |
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| 出典メモ | uspto-grants-2014_11 |
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