関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Anisole | HCID 7519 | — |
| 反応物 | HCID 178427556 | HCID 178427556 | — |
| 触媒 | Ethyl methyl sulfide | HCID 12230 | — |
| 溶媒 | Diethylether hexane | HCID 21584099 | — |
| 生成物 | HCID 178512906 | HCID 178512906 | 60% |
反応手順
A 100 mg portion of Boc-(D)-Arg(Cbz2)-Gly-Arg(Tos)-Thiazole, 1 mL of anisole and 4 drops of MeSEt were placed in HF-cleavage vessel and cooled under liquid N2. HF (10 mL) was then condensed into the reaction mixture and stirred at 0° C. for 1.25 h. HF was removed under vacuum to give a gum-like residue which was titrated with 20 mL of 50% Et2O-hexane and the organic wash removed by filtration. The gum residue was dissolved in 30 mL of 30% aq. HOAc and filtered through the above sintered funnel. The filtrate was lyophilized to give a powder which was purified by RP-HPLC to give 28 mg (60% yield) of (D)-Arg-Gly-Arg-thiazole. FAB-MS (M+H)+ =455.2
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06069130 |
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| 出典データセット | uspto-grants-2000_05 |
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| ORD ID | ord-283db2cfbe884f068a53863e057d09e1 |
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| 出典メモ | uspto-grants-2000_05 |
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