関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tryptamine | HCID 1150 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | HCID 178505057 | HCID 178505057 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | HCID 178505055 | HCID 178505055 | — |
反応手順
A solution of 0.3 g (0.45 mmol) of trans-4-[4-(benzyl{(2S)-3-[4-(benzyloxy)-3-[(methylsulfonyl)amino]phenoxy]-2-hydroxypropyl}amino)cyclohexyl]benzoic acid (preparation 3), of 0.78 g (0.91 mmol) of 1-hydroxybenzotriazole, of 0.175 g (0.91 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide, of 0.19 ml of triethylamine and of 0.138 g (0.86 mmol) of tryptamine in a mixture of 4 ml of dichloromethane and 0.8 ml of acetonitrile is stirred for 24 h. The solvents are evaporated under reduced pressure. Dichloromethane and water are added and the organic phase is washed three times with water. The organic phases are dried over magnesium sulfate and concentrated under reduced pressure. The title compound is obtained in the form of a white solid (0.246 g, 58%) after purification on silica gel (eluent: heptane/ethyl acetate 60/40 for 10 min, 60/40 to 40/60 in 10 min and then 40/60 for 20 min gradient). [M+H+]=801.6
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07453010B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-ea988d814a9d4954a72630fd61008ae2 |
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| 出典メモ | uspto-grants-2008_11 |
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