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Tert-Butylamine → N-tert-butyl-4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridin-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tert-Butylamine | HCID 6385 | — |
| 反応物 | Toluene-p-sulphonic anhydride | HCID 77773 | — |
| 反応物 | 4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridine 1-oxide | HCID 67184479 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | (Trifluoromethyl)benzene | HCID 7368 | — |
| 生成物 | N-tert-butyl-4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridin-2-amine | HCID 67185904 | 75% |
反応手順
580 mg (1.44 mmol) of 4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridine 1-oxide were suspended in a mixture of 16 ml of trifluoromethylbenzene and 4 ml of dry dichloromethane and 756 μl of tert-butylamine were added. At 0° C. 936 mg (7.2 mmol) of p-toluensulfonic anhydride were added. After 6 hours under stirring in the same conditions the solvent was removed under reduced pressure, the residue partitioned between dichloromethane and water, the organic layer dried over sodium sulphate and evaporated. The crude was then purified by flash-chromatography on a silica gel column (CH2Cl2-CH3COCH3 19/1), giving 500 mg (75%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08946250B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-9fa05e8f432c4aaaac93fd42ead53fa4 |
| 出典メモ | uspto-grants-2015_02 |