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Ethylmorpholine → Z-Ile-Phe-OBut
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylmorpholine | HCID 7525 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | N-[(Phenylmethoxy)carbonyl]-L-isoleucine | HCID 2724772 | — |
| 反応物 | tert-butyl (2S)-2-amino-3-phenylpropanoate | HCID 6931633 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Z-Ile-Phe-OBut | HCID 131713277 | — |
反応手順
1.3 ml of N-ethylmorpholine are added to the solution of 2.65 g of Z-Ile-OH, 2.58 g of H-Phe-OBut and 1.35 g of HOBt in 30 ml of dimethylformamide and 2.2 g of DCC are added to 0° C. The mixture is allowed to stand for 1 hour at 0° C. and overnight at room temperature. On the following day the precipitate is filtered off and the filtrate is concentrated. The residue is partitioned between ethyl acetate and water. The ethyl acetate phase is extracted by shaking with 20 ml of saturated NaHCO3 solution, 20 ml of K2SO4 /KHSO4 solution and 20 ml of NaHCO3 solution and is dried over Na2SO4 and concentrated. The product crystallizes from petroleum ether. Yield 3.7 g, melting point 122°-125°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04420424 |
| 出典データセット | uspto-grants-1983_12 |
| ORD ID | ord-a9eaf38e2fd04680b6ed72562a431c04 |
| 出典メモ | uspto-grants-1983_12 |