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Triethylamine → 3-(Benzenesulfonyl-benzyl-amino)-N-(1H-indazol-6-yl)-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1H-Indazol-6-amine | HCID 81423 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 3-(Benzenesulfonyl-benzyl-amino)-benzoic acid | HCID 67310950 | — |
| 反応物 | HCID 178418395 | HCID 178418395 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(Benzenesulfonyl-benzyl-amino)-N-(1H-indazol-6-yl)-benzamide | HCID 46182505 | 45.7% |
反応手順
A solution of 3-(benzenesulfonyl-benzyl-amino)-benzoic acid (25 mg, 0.068 mmol), 6-amino-1H-indazole (18 mg, 0.136 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (15 mg, 0.075 mmol), mercaptobenzothiazole (2 mg, 0.007 mmol) and triethylamine (24 μl, 0.17 mmol) in dry acetonitrile (2 ml) were stirred at room temperature for 15 hrs. The reaction mixture was quenched with water (10 ml) and extracted with dichloromethane (3×7 ml). The organics were combined, dried (PTFE frit) and concentrated in vacuo. The crude residue was purified by preparative TLC (10% diethyl ether in dichloromethane) to afford the title compound as a brown solid (15 mg, 45%). HPLC retention time 5.80 min. Mass spectrum (ES+) m/z 483 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447033B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-e00d585c5899472b8e024f7de6bf0a1a |
| 出典メモ | uspto-grants-2016_09 |