関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | Ethyl L-phenylalaninate hydrochloride | HCID 165085 | — |
| 反応物 | L-Threonine, N-[(1,1-dimethylethoxy)carbonyl]-O-(phenylmethyl)- | HCID 1549483 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Boc-Thr(Bzl)-Phe-OEt | HCID 131712163 | 81% |
反応手順
To 200 ml of methylene chloride, were added 31.0 g of Boc-Thr(Bzl)-OH and 27.6 g of Phe-OEt.HCl, and 18.3 ml of WSC were added to the mixture under cooling at 0°--5° C., which was then subjected to stirring for 2 hours at 0°--5° C. then for 18 hours at room temperature. The methylene chloride in the reaction solution was exchanged with ethyl acetate and the exchanged solution was washed successively with 1 N HCl, 5% aqueous NaHCO3 solution and water and dried over MgSO4. The organic layer was concentrated and the produced material was crystallized from hexane, which gave 39.0 g (yield=81%) of the title compound. m.p. 99°-100.5° C. [α]D25 +6.2° (C 2.7, DMF). Analysis--Calculated for C27H36O6N2 : C, 66.92; H, 7.49; N, 5.78. Found: C, 66.91; H, 7.57; N, 5.75.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04261885 |
|---|
| 出典データセット | uspto-grants-1981_04 |
|---|
| ORD ID | ord-a7d1204e4ef04932a9986867138df29c |
|---|
| 出典メモ | uspto-grants-1981_04 |
|---|
