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Ethyl Acetate → 2-[4-(1-Benzothien-2-ylmethyl)-1-piperazinyl]benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Methanesulfonic anhydride | HCID 81560 | — |
| 反応物 | N-(2-Cyanophenyl)piperazine | HCID 2735875 | — |
| 反応物 | 2-(Hydroxymethyl)benzo[b]thiophene | HCID 2776335 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-[4-(1-Benzothien-2-ylmethyl)-1-piperazinyl]benzonitrile | HCID 9996948 | — |
反応手順
The product from Example 8A (150 mg 0.9 mmol), methane sulfonic anhydride (159 mg, 0.9 mmol), and D1 EA (475 μL 2.7 mmol) were combined. After stirring, 2-(1-piperazinyl)benzonitrile (181 mg, 1.0 mmol) in 2 ml DCM was also combined and stirred at room temperature for 18 hours. The mixture was concentrated and the residue was taken up in hot methanol. The methanol was filtered and the filter cake washed with cold methanol to provide the title compound. 1H NMR (300 MHz, CDCl3) δ 2.69 (m, 4H) 3.04 (s, 4H) 3.76 (m, 4H) 3.86 (s, 1H) 6.74 (m, 2H) 7.29 (m, 3H) 7.75 (m, 1H); (ESI) m/z 334 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07470691B2 |
| 出典データセット | uspto-grants-2008_12 |
| ORD ID | ord-c9a658dc3dd743c4a7da7ed15e88db60 |
| 出典メモ | uspto-grants-2008_12 |