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Water → Fmoc-N-Me-Val-N-Me-Tyr(Bzl)-NH2
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | (2S)-2-((((9H-fluoren-9-yl)methoxy)carbonyl)(methyl)amino)-3-methylbutanoic acid | HCID 978328 | — |
| 反応物 | N-Me-Tyr(Bzl)-NH2 | HCID 131723958 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Fmoc-N-Me-Val-N-Me-Tyr(Bzl)-NH2 | HCID 131723957 | 95% |
反応手順
To a solution of N-Me-Tyr(Bzl)—NH2 (329 mg, 1.16 mmol) in THF (15 ml), Fmoc-N-Me-Val-OH (533 mg, 1.51 mmol), CMPI (415 mg, 1.62 mmol) and TEA (0.323 ml, 2.32 mmol) were added under cooling with ice, followed by stirring for 4 hours at room temperature. The reaction mixture was mixed with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate and evaporated to remove the solvent under-reduced pressure; the thus obtained residue was subjected to silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=2:1) to give the titled compound (680 mg, 95%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06586630B1 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-7c8211838e684a638f80eb07e6081b58 |
| 出典メモ | uspto-grants-2003_07 |