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Trifluoroacetic acid → [2-(Ethoxycarbonyl)-1-benzothien-6-yl]malonic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Di-tert-butyl [2-(ethoxycarbonyl)-1-benzothien-6-yl]malonate | HCID 59424236 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | [2-(Ethoxycarbonyl)-1-benzothien-6-yl]malonic acid | HCID 59424242 | — |
反応手順
Di-tert-butyl[2-(ethoxycarbonyl)-1-benzothien-6-yl]malonate (0.873 g, 2.08 mmol) was dissolved in DCM (5 mL) and TFA (5 mL) was added. The solution was stirred at room temperature for 2 hours. The solvent was removed in vacuo and the residue partitioned between saturated NaHCO3-EtOAc. The aqueous phase was acidified with 2N HCl and extracted with EtOAc. The combined organic extracts were dried over MgSO4 and concentrated in vacuo to give the product (white solid). 1H NMR (DMSO-d6) δ 13.10 (br s, 2H), 8.17 (s, 1H), 8.03 (s, 1H), 7.98 (d, J=8.4 Hz, 1H), 7.47 (dd, J=8.4, 1.8 Hz, 1H), 4.83 (s, 1H), 4.33 (q, J=7.2 Hz, 2H), 1.32 (t, J=7.2 Hz, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07834034B2 |
| 出典データセット | uspto-grants-2010_11 |
| ORD ID | ord-8067dd964e7242a0977b5bc68225919a |
| 出典メモ | uspto-grants-2010_11 |