関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | D-Alanine | HCID 71080 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4'-[(Benzofuran-2-carbonyl)-amino]-biphenyl-4-sulfonyl chloride | HCID 86058865 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-({4'-[(1-benzofuran-2-ylcarbonyl)amino]-1,1'-biphenyl-4-yl}sulfonyl)-D-alanine | HCID 68715986 | — |
反応手順
To a solution of D-alanine (0.15 mmol, 14 mg) in water (0.5 mL) and DMF (0.1 mL) was added N,N-diisopropylethylamine (52 uL, 0.3 mmol) and 4′-[(benzofuran-2-carbonyl)-amino]-biphenyl-4-sulfonyl chloride (0.1 mmol, 41 mg) as a solution in acetonitrile (0.4 mL). The resulting solution was shaken at room temperature for 4 hours and purified by semi-preparative RP-HPLC (Gilson Preparative HPLC conditions: Gilson Preparative HPLC system; YMC Pro C18, 20 mm×50 mm ID, 5 uM column; 2 mL injection; Solvent A: 0.02% TFA/water; Solvent B: 0.02% TFA/acetonitrile; Gradient: Time 0: 95% A; 2 min: 95% A; 14 min: 10% A, 15 min: 10% A, 16 min: 95% A; Flow rate 22.5 mL/min; Detection: 254 nm DAD.) to provide N-({4′-[(1-benzofuran-2-ylcarbonyl)amino]-1,1′-biphenyl-4-yl}sulfonyl)-D-alanine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07420001B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-8c0cc42172bb4ebc9c2334034adf4885 |
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| 出典メモ | uspto-grants-2008_09 |
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