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Triethylamine → 5-(N-(3-((N-(Biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxyphenylsulfonamido)methyl)benzyl)sulfamoyl)-2-methylbenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-(Chlorosulfonyl)-2-methylbenzoic acid | HCID 308449 | — |
| 反応物 | N-(3-(Aminomethyl)benzyl)-N-(biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxybenzenesulfonamide | HCID 58531388 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-(N-(3-((N-(Biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxyphenylsulfonamido)methyl)benzyl)sulfamoyl)-2-methylbenzoic acid | HCID 66616505 | 58.1% |
反応手順
To a solution of N-(3-(aminomethyl)benzyl)-N-(biphenyl-4-ylmethyl)-3,5-dichloro-2-hydroxybenzenesulfonamide (50 mg, 0.095 mmol) and Et3N (0.13 mL) in CH2Cl2 (4 mL) was added a solid of 5-(chlorosulfonyl)-2-methylbenzoic acid (22.24 mg, 0.095 mmol) at rt and it was stirred at it for 70 min. Direct purification of the mixture after concentration by prep HPLC provided the desired product (40 mg, 58.1%) as a white solid after lyophilization. 1H NMR (CD3OD): δ 8.17 (d, J=2.0 Hz, 1H), 7.93 (dd, J=8.3, 2.2 Hz, 1H), 7.56˜6.90 (m, 15H), 6.76 (s, 1H), 4.34 (s, 2H), 4.31 (s, 2H), 3.87 (s, 2H), 2.52 (s, 3H); MS (ESI): (M+H)+=725.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08501992B2 |
| 出典データセット | uspto-grants-2013_08 |
| ORD ID | ord-70127a297d67473496f5e005ad3600ef |
| 出典メモ | uspto-grants-2013_08 |