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4-Methylmorpholine → N-benzyloxycarbonyl-L-leucinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | Isobutyl chloroformate | HCID 62365 | — |
| 反応物 | Leucine, N-carboxy-, N-benzyl ester, L- | HCID 74840 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-benzyloxycarbonyl-L-leucinamide | HCID 69952024 | 100.2% |
反応手順
To a stirring solution of N-benzyloxycarbonyl-L-leucine (4.6 g, 17.3 mmol) in THF, cooled to -40° C., was added N-methylmorpholine (3.68 g, 36.4 mmol; 4.0 mL) and isobutyl chloroformate (2.37 g, 17.3 mmol; 2.25 mL). After stirring for 15 min, ammonia was bubbled through the solution for 5 min. The solution was warmed to room temperature, evaporated, and the residue was dissolved in ethyl acetate, washed with 0.1 N Hcl, and saturated brine, then dried (MgSO4), filtered and evaporated to dryness to give the title compound as a white solid (4.58 g, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05998470 |
| 出典データセット | uspto-grants-1999_12 |
| ORD ID | ord-de3741207e3a4828960a16333862fcc4 |
| 出典メモ | uspto-grants-1999_12 |