関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 3-Aminobenzenesulfonic acid | HCID 8474 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Boc-Ser-Otbu | HCID 7019054 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | O-{[(3-sulfophenyl)amino]carbonyl}-L-serine | HCID 45275682 | 0.6% |
反応手順
Boc-Ser-OtBu (200 mg, 0.77 mmol) was dissolved in 3 mL of methylene chloride and cooled down to 0° C. N,N′-carbonyldiimidazole (124 mg, 0.77 mmol) was added thereto and stirred at room temperature for 2 hours. After removing a solvent, 3-aminobenzenesulfonic acid (132.6 mg, 0.77 mmol), 2 mL of DMF and 0.4 mL of diisopropylethylamine were added thereto and stirred at 70° C. overnight. After removing a solvent, the mixture was purified in accordance with the purification process A to obtain an intermediate. The obtained intermediate was dissolved in 1 mL of TFA and stirred at room temperature for 2 hours. After removing a solvent, purification was conducted in accordance with the purification process A to obtain a title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09174932B2 |
|---|
| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-acb1354df1474281a1e3ac071f222f3f |
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| 出典メモ | uspto-grants-2015_11 |
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