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Potassium Carbonate → Benzo[b]thiophene-2-carboxylic acid, 3-amino-6-chloro-, methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl Thioglycolate | HCID 12185 | — |
| 反応物 | 4-Chloro-2-nitrobenzonitrile | HCID 96924 | — |
| 反応物 | Ethyl acetate hexane | HCID 21226206 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Benzo[b]thiophene-2-carboxylic acid, 3-amino-6-chloro-, methyl ester | HCID 14916787 | 31% |
反応手順
2-nitro-4-chlorobenzonitrile (1.94 g, 10.6 mmol) was treated with 1 eq of ethyl thioglycolate and 1 eq potassium carbonate in EtOH as described in Example 41A to give after chromatography (4:1 hexane/EtOAc) the title compound in 31% yield. 1H NMR (300 MHz, CDCl3) d 1.38 (t, J=7 Hz, 3H), 4.36 (q, J=7 Hz, 2H), 5.85 (bs, 2H), 7.33 (dd, J=9,2 Hz, 1H), 7.54 (d, J=9 Hz; 1H), 7.1 (d, J=2 Hz, 1H). MS (DCI/NH3) m/e 256 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05597823 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-6bc4b181c0634fd8a28e20f02217f777 |
| 出典メモ | uspto-grants-1997_01 |