関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Propanol, 1-amino-2-methyl- | HCID 95102 | — |
| 反応物 | 5-Fluoro-2-nitroanisole | HCID 2779250 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(3-Methoxy-4-nitrophenylamino)-2-methylpropan-2-ol | HCID 65109358 | — |
反応手順
A 20 mL reaction vial equipped with a stir bar was charged with 4-fluoro-2-methoxy-1-nitrobenzene (0.5 g, 2.92 mmol), 1-amino-2-methylpropan-2-ol (0.313 g, 3.51 mmol), N-methyl-2-pyrrolidinone (7.3 mL) and Hunig's base (N,N-diisopropylethylamine) (0.76 g, 5.84 mmol). The vessel was sealed and the reaction was heated on a thermal block at 80° C. for 24 hours. The reaction was cooled to ambient temperature, treated with water (40 mL) and extracted with ethyl acetate (3×60 mL). The combined organic layers were washed with brine (25 mL), dried over Na2SO4, filtered, and concentrated. The concentrate was purified by flash chromatography on a 10 g silica gel column with 1% methanol/CH2Cl2 to provide the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08536180B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-c98108077fe4464e8dc39edb59beb0a9 |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|