関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2'-Dithiodibenzoyl chloride | HCID 88164 | — |
| 反応物 | Methyl 3-amino-2-thiophenecarboxylate | HCID 89652 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3,3'-[Dithiobis(2,1-phenylenecarbonylimino)]bis-2-thiophenecarboxylic acid, dimethyl ester | HCID 86751259 | 59% |
反応手順
A solution of 2,2'-dithiobisbenzoyl chloride (2.00 g, 5.83 mmol) in 50 mL of dichloromethane was added to a solution of methyl 3-amino-2-thiophenecarboxylate (1.82 g, 11.6 mmol) in 14 mL of pyridine at 23° C. The reaction mixture was stirred for 18 hours at 23° C. under nitrogen atmosphere. The precipitate formed was collected by filtration, then triturated with 5% aqueous HCl and washed with water to yield the crude product. The crude material was recrystallized first from ethanol, then from acetonitrile-DMF to yield 2.0 g of the title compound, mp 250°-252° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05734081 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-b718485e058f488da242388c9e90b503 |
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| 出典メモ | uspto-grants-1998_03 |
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