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Hydrochloric Acid → Boc-D-Trp-D-Trp-NH2
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Methylmorpholine | HCID 7972 | — |
| 反応物 | N-((tert-Butoxy)carbonyl)-D-tryptophan | HCID 111050 | — |
| 反応物 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 反応物 | D-tryptophanamide | HCID 688582 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Boc-D-Trp-D-Trp-NH2 | HCID 131724766 | 99.8% |
反応手順
In 10 ml of DMF, HCl, H-D-Trp-NH2 (8.9 mmol; 1 eq.), Boc-D-Trp-OH (2.98 g; 9.8 mmol; 1.1 eq.), NMM (2.26 ml; 2.1 eq.) and BOP (4.33 g; 1.1 eq.) were added successively. After 1 hr, the mixture was diluted with ethyl acetate (100 ml) and washed with saturated aqueous sodium hydrogen carbonate (200 ml), aqueous potassium hydrogen sulfate (200 ml, 1M), and saturated aqueous sodium chloride (100 ml). The organic layer was dried over sodium sulfate, filtered and the solvent removed in vacuo to afford 4.35 g of Boc-D-Trp-D-Trp-NH2 as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07297681B2 |
| 出典データセット | uspto-grants-2007_11 |
| ORD ID | ord-dc9573695ab041c091636eb7de7708f7 |
| 出典メモ | uspto-grants-2007_11 |