関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Methylpiperazine, (R)- | HCID 7330434 | — |
| 反応物 | 1H-Benzimidazole, 2,7-dichloro-5-(trifluoromethyl)- | HCID 66937336 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | HCID 178461512 | HCID 178461512 | — |
反応手順
A mixture of 2,4-dichloro-6-trifluoromethyl-1H-benzoimidazole (0.51 g, 2 mmol, Example 5b), (R)-(−)-2-methylpiperazine (0.25 g. 2.5 mmol) and N,N-diisopropylethylamine (0.5 mL, 2.9 mmol) in NMP (5 mL) was heated at 120° C. for 16 h. The reaction mixture was cooled to room temperature, diluted with water (10 mL) and extracted with EtOAc (2×20 mL). The combined organic phases were washed with brine (10 mL), dried over Na2SO4 and filtered. The filtrate was concentrated in vacuo and the residue was purified by silica gel chromatography, eluting with 10% MeOH in dichloromethane to give the title compound as a light-yellow solid. MS (ESI, pos. ion) m/z: 319 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07582761B2 |
|---|
| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-89b01c30d9f344f7a4ca34bf0698a701 |
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| 出典メモ | uspto-grants-2009_09 |
|---|
