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Potassium Carbonate → phenyl 3-tert-butyl-1-methyl-1H-pyrazol-5-ylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 3-tert-Butyl-1-methyl-1H-pyrazol-5-amine | HCID 2735287 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | phenyl 3-tert-butyl-1-methyl-1H-pyrazol-5-ylcarbamate | HCID 46196890 | 31% |
反応手順
According to the procedure described in Example 161C, to a suspension of 3-tert-butyl-1-methyl-1H-pyrazol-5-amine (1.0 g, 6.5 mmol) and K2CO3 (1.17 g, 8.5 mmol) in THF (15 mL) was added phenyl chloroformate (1.12 g, 7.2 mmol). The crude product was purified by silica gel chromatography with 0-50% EtOAc/hexane as eluants to afford phenyl 3-tert-butyl-1-methyl-1H-pyrazol-5-ylcarbamate as solid (0.53 g, 31%). 1H NMR (300 MHz, DMSO-d6) δ 10.2 (s, 1H), 7.43 (m, 2H), 7.25 (m, 3H), 6.06 (s, 1H), 3.66 (s, 3H), 1.25 (s, 9H); LC-MS (ESI) m/z 274 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08969587B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-221f88d0327348bfbd819cb5ad7ae033 |
| 出典メモ | uspto-grants-2015_03 |