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Hydrochloric Acid → Thiophene-2,5-dicarboxylic acid di-1,3-benzodioxol-5-ylmethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2,5-Thiophenedicarboxylic acid | HCID 20273 | — |
| 反応物 | 1,3-Benzodioxole, 5-(chloromethyl)- | HCID 88713 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Thiophene-2,5-dicarboxylic acid di-1,3-benzodioxol-5-ylmethyl ester | HCID 69693184 | — |
反応手順
Cesium carbonate (4.7 g, 14.4 mmol) was added to a stirred solution of 2,5-thiophenedicarboxylic acid in dimethylformamide (35 mL) under an inert atmosphere at room temperature. After 5 minutes, a solution of 3,4-methylenedioxybenzyl chloride in dichloromethane (3.7 mL, 14.3 mmol) was added. After 24 hours the mixture was stirred into water (150 mL) and acidified with dilute aqueous HCl. After several hours, the precipitate was filtered off, rinsed with water, and dried to afford 0.6 g of thiophene-2,5-dicarboxylic acid di-1,3-benzodioxol-5-ylmethyl ester. Recrystallization of a sample from ethanol gave product with a mp 141-148° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06924276B2 |
| 出典データセット | uspto-grants-2005_08 |
| ORD ID | ord-e262d475e39c4c9497b1e3db39202161 |
| 出典メモ | uspto-grants-2005_08 |