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Diisopropylethylamine → 4'-Fluoro-biphenyl-4-carboxylic acid {2-[(2-dimethylamino-ethyl)-methyl-amino]-benzothiazol-6-yl}-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-(4-Fluorophenyl)benzoic acid | HCID 2782689 | — |
| 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 | N2-(2-Dimethylamino-ethyl)-N2-methyl-benzothiazole-2,6-diamine | HCID 55226563 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4'-Fluoro-biphenyl-4-carboxylic acid {2-[(2-dimethylamino-ethyl)-methyl-amino]-benzothiazol-6-yl}-amide | HCID 11597542 | 60% |
反応手順
Prepare according to Method A, using 4-(4-fluorophenyl)benzoic acid (572 mg, 2.65 mmol), HATU (1.06 g, 2.79 mmol), N2-(2-dimethylamino-ethyl)-N2-methyl-benzothiazole-2,6-diamine (500 mg, 2.00 mmol), DIEA (1.15 mL, 6.60 mmol), and a chromatography gradient of MeOH in CH2Cl2 (7-17%) to afford the title compound (535 mg, 60%). mass spectrum (m/e): 449.0 [M+H]. 1H NMR (400 MHz, DMSO-d6): δ 10.29 (s, 1H), 8.26 (d, 1H, J=2.2 Hz), 8.06 (d, 2H, J=8.4 Hz), 7.84-7.78 (m, 4H), 7.57 (dd, 1H, J=8.8, 2.2 Hz), 7.41 (d, 1H, J=8.8 Hz), 7.34 (t, 2H, J=8.8 Hz), 3.61 (t, 2H, J=6.8 Hz), 3.14 (s, 3H), 2.52 (m, 2H), 2.20 (s, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07838543B2 |
| 出典データセット | uspto-grants-2010_11 |
| ORD ID | ord-66b949c7edf14227a9ca2abc9e96de18 |
| 出典メモ | uspto-grants-2010_11 |