関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-(3-Cyanophenyl)-1-(3,3-diphenylpropyl)-1-(2-morpholin-4-ylethyl)urea | HCID 16737642 | — |
| 反応物 | Diethyldithiophosphate | HCID 53249491 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-[3-(3,3-Diphenylpropyl)-3-(2-morpholin-4-ylethyl)ureido]thiobenzamide | HCID 16736914 | — |
反応手順
70 mg (0.15 mmol, 1 eq.) of 3-(3-cyanophenyl)-1-(3,3-diphenylpropyl)-1-(2-morpholin-4-ylethyl)urea (obtained in Example 19) are dissolved in 0.5 mL of THF under argon. 142 μL (0.90 mmol, 6 eq.) of diethyldithiophosphate and 50 μL (0.01 mmol, 0.1 eq.) of water are added. The mixture is stirred for 27 hours at 40° C. Water is added to the medium and the aqueous phase is extracted with dichloromethane, washed twice with water then brine, dried over MgSO4, filtered and concentrated. The oil obtained is subjected to chromatography over silica gel (eluent: 97/3 dichloromethane/methanol) in order to obtain the expected product in the form of a yellow powder (55 mg, yield=73%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07875609B2 |
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| 出典データセット | uspto-grants-2011_01 |
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| ORD ID | ord-34a646655879462d8d9a6928ed341f88 |
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| 出典メモ | uspto-grants-2011_01 |
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