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4-Piperidinecarboxylic acid → 1,1'-[Dithiobis(2,1-phenylenecarbonyl)]bis-4-piperidine carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Piperidinecarboxylic acid | HCID 3773 | — |
| 反応物 | N-Trimethylsilyl-N-methylacetamide | HCID 81953 | — |
| 反応物 | 2,2'-Dithiodibenzoyl chloride | HCID 88164 | — |
| 触媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1,1'-[Dithiobis(2,1-phenylenecarbonyl)]bis-4-piperidine carboxylic acid | HCID 18935289 | — |
反応手順
Isonipecotic acid (4-piperidinecarboxylic acid) (0.76 g, 6 mmol), N-methyl-N-trimethylsilylacetamide and 3 drops of pyridine were stirred at room temperature for 2 hours. This suspension was added to a filtered solution of 2,2'-dithiobisbenzoyl chloride (1.0 g, 3.0 mmol) in 15 mL of dichloromethane. The solvent was removed after 18 hours and the residue was triturated with 1N HCl. The acid was decanted and the residue was dissolved in acetonitrile. After standing for 24 hours a precipitate formed. The solid was collected and dried to give 0.56 g of the title compound, mp>250° C.;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05734081 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-90022719d27c459586f6b49166817b5d |
| 出典メモ | uspto-grants-1998_03 |