関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | tert-butyl (S)-(1-(4-methyl-2'-(trifluoromethyl)-[3,4'-bipyridin]-6-yl)ethyl)carbamate | HCID 90451687 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (S)-1-(4-Methyl-2'-(trifluoromethyl)-[3,4'-bipyridin]-6-yl)ethan-1-amine | HCID 90423562 | 99.7% |
反応手順
To a solution of (S)-tert-butyl(1-(4-methyl-2′-(trifluoromethyl)-[3,4′-bipyridin]-6-yl)ethyl)carbamate (200 mg, 0.524 mmol) in DCM (2 ml) at −78° C. was added trifluoroacetic acid (2 mL, 12.98 mmol). The solution was stirred at r.t. for 1 hr. The mixture was concentrated, diluted with 10 mL DCM and stirred with solid MP-carbonate to remove TFA. Filtered and concentrated to give 147 mg (S)-1-(4-methyl-2′-(trifluoromethyl)-[3,4′-bipyridin]-6-yl)ethanamine as a light brown sticky oil. MS m/z 282.1 (M+H). Rt=0.85 min. (Column: XBridge C18 3.5 um 2.1×50 mm. Solvent A: 2% Acetonitrile, 3.75 mM Ammonium Acetate, Water. Solvent B: Acetonitrile. Gradient: 5-95% B over 1.70 min. Flow rate: 2 mL/min.) The crude product was used to 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 | US09434719B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-f79611c2ca09411da2304cdfa819ecd5 |
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| 出典メモ | uspto-grants-2016_09 |
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