関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | phenyl N-(1,3-thiazol-2-yl)carbamate | HCID 651148 | — |
| 反応物 | HCID 68704951 | HCID 68704951 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | HCID 59251035 | HCID 59251035 | 29% |
反応手順
A mixture of 3-(1-(4-fluorophenyl)-1H-indazol-5-yl)-2,2,3-trimethylbutan-1-amine (10 mg, 0.031 mmol), phenyl thiazol-2-ylcarbamate (15 mg, 0.068 mmol), diisopropylethylamine (0.1 mL), and anhydrous acetonitrile (0.1 mL) was stirred under nitrogen at 80° C. till the reaction completed (ca 30 min) The mixture was dissolved in methanol and TFA. Purification using reverse phase HPLC (YMC S5 20×100 mm, 10 min. run, solvent A: 10% MeOH: 90% H2O: 0.1% TFA, solvent B: 90% MeOH, 10% H2O, 0.1% TFA) gave the title compound (4 mg, 0.009 mmol, 29% yield) as a white solid. MS found: (M+H)+=452. 1H-NMR (400 MHz, CHLOROFORM-d) δ ppm 8.16 (s, 1 H) 7.79 (s, 1 H) 7.69 (dd, J=8.90, 4.83 Hz, 2 H) 7.60 (d, J=9.10 Hz, 1 H) 7.52 (dd, J=9.10, 1.70 Hz, 1 H) 7.21-7.31 (m, 3 H) 6.91 (d, J=4.07 Hz, 1 H) 5.56 (t, J=6.00 Hz, 1 H) 3.28 (d, J=6.10 Hz, 2 H) 1.52 (s, 6 H) 0.96 (s, 6 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08198311B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-9399435b433a47249ae04f7a44bed427 |
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| 出典メモ | uspto-grants-2012_06 |
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