関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | (R)-2-(((S)-2-cyano-1-(4-methoxyphenyl)propan-2-yl) amino)-2-phenylacetamide | HCID 67200502 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-[(R)-(Carbamoylphenylmethyl)-amino]-3-(4-methoxyphenyl)-2-(S)-methylpropionamide | HCID 67167012 | — |
反応手順
To a 500 mL flask were added nitrile 2 (10.0 g, 30.95 mmol) and CH2Cl2 (130 mL). The solution was cooled to −10° C. and H2SO4 (10 mL) was added dropwise over 15 min. The mixture was stirred for 2 h at 0° C. Ice (200 g) was added and the mixture was stirred for 1 h. The mixture was basified with 32% aq NH3 to pH 8-9, EtOAc (400 mL) was added and the phases were separated. The aqueous phase was extracted with EtOAc (2×250 mL). The combined organic phases were dried over MgSO4 and were concentrated to provide 3 (11.1 g (9.99 g theoretical, the sample contains 10% w/w of EtOAc by NMR) 94%, 92.9% chemical purity, 97% de by HPLC/MS) as a white solid. HPLC/MS tR=3.04 min; m/z=342.1 (M+1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08841486B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-5b7042aa79594fc7986d5d8042e1dca5 |
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| 出典メモ | uspto-grants-2014_09 |
|---|
