関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Iodobenzene diacetate | HCID 76724 | — |
| 反応物 | N2-((tert-Butoxy)carbonyl)-L-asparagine | HCID 82035 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Boc-Dap-OH | HCID 2755946 | 62% |
反応手順
A slurry of N-Boc-L-asparagine (5.00 g, 21.5 mmol), EtOAc (24 mL), acetonitrile (24 mL), water (12 mL), and PIDA (8.32 g, 25.8 mmol) was cooled and stirred at 16° C. for 30 min. The temperature was then allowed to reach 20° C., and the reaction was stirred until completion (ca. 4 h). The mixture was cooled to 0° C. and filtered. The filter cake was washed with EtOAc (10 mL) and dried in vacuo to give 1 (2.73 g, 62% yield). 1H NMR (CD3OD and a drop of TFA) δ4.05 (1H), 3.20-3.08 (2H), 1.45 (9H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09394338B2 |
|---|
| 出典データセット | uspto-grants-2016_07 |
|---|
| ORD ID | ord-04c0041e90df4b09b95c11870fd224cd |
|---|
| 出典メモ | uspto-grants-2016_07 |
|---|
