化工社化工社 化学情報印刷レポート · 研究参考用
Benzenesulfonic acid, 3-amino-5-chloro-4-methyl- → N5-(3-chloro-2-methyl-5-sulfophenyl)-L-glutamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzenesulfonic acid, 3-amino-5-chloro-4-methyl- | HCID 80806 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | HOAt | HCID 181649 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 反応物 | Boc-Glu-OtBu hydrochloride | HCID 131731743 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | N5-(3-chloro-2-methyl-5-sulfophenyl)-L-glutamine | HCID 45275582 | — |
反応手順
After 2 ml of DMF and 0.52 ml (3 mmol) of DIEA were added to 303 mg (1 mmol) of Boc-Glu-OtBu hydrochloride, 221 mg (1 mmol) of 3-amino-5-chloro-4-methylbenzenesulfonic acid, 160 mg (1.3 mmol) of HOAt and 410 mg (1.3 mmol) of HATU, the mixture was stirred at room temperature overnight. The reaction solution was diluted in water-acetonitrile and purified in accordance with the purification step A to give the protected form of the product. The protected product obtained was dissolved in 5 ml of trifluoroacetic acid and stirred for 2 hours. After the solvent was removed by distillation, the mixture was purified in accordance with the purification step A to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08877739B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-514188b64829444189e1edd87a4f6c62 |
| 出典メモ | uspto-grants-2014_11 |