関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Tert-Butylaniline | HCID 69861 | — |
| 反応物 | 2,2'-Dithiodibenzoyl chloride | HCID 88164 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(4-tert-butylphenyl)-2-[[2-[(4-tert-butylphenyl)carbamoyl]phenyl]disulfanyl]benzamide | HCID 465328 | 12.1% |
反応手順
A solution of 2,2'-dithiobisbenzoyl chloride (1.20 g, 3.50 mmol) in 25 mL of dichloromethane was added to a solution of 4-tert-butylaniline (1.04 g, 6.99 mmol) in 8 mL of pyridine at 23° C. The reaction mixture was stirred for 18 hours at 23° C. under nitrogen atmosphere. The mixture was concentrated, the residue triturated with 5% aqueous HCl, and the resulting solid was collected by filtration and washed with water to yield the crude product. The crude material was recrystallized from ethyl ether-ethanol to yield 0.24 g of the title compound, mp 135°-138° 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-633d84603ffe4743a9aba35936f4eeaa |
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| 出典メモ | uspto-grants-1998_03 |
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