関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1-Bromo-4-tert-butylbenzene | HCID 77595 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | HCID 178506930 | HCID 178506930 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 4-Tert-Butylaniline | HCID 69861 | 72% |
反応手順
(CyPF-t-Bu)PdCl2 (7.30 mg, 1.00×10−2 mmol), LiNH2 (0.230 g, 10.0 mmol) and 4-t-butyl-1-bromobenzene (0.213 g, 1.00 mmol) were weighed into a 24 mL vial. DME (20.0 mL) was then added. The vial was sealed with a cap containing a PTFE septum, and the reaction mixture was stirred for 24 h at 80° C. The reaction mixture was allowed to cool to room temperature before pouring into ice water (20.0 mL). To this mixture was added HCl aqueous solution (10.0 mL, 1.0 M). The mixture was stirred at room temperature for 5 min and was then neutralized with a saturated solution of NaHCO3 (5.00-10.0 mL). After extraction with CH2Cl2 (3×20.0 mL), the organic layer was separated and dried over MgSO4. The solvent was evaporated, and the crude product isolated by eluting with hexane/ethyl acetate (80/20) to give 107.0 mg (72%) of 4-t-butylaniline as a pale yellow liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08058477B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-a97113e187f54bafb55dba5681d14069 |
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| 出典メモ | uspto-grants-2011_11 |
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