Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tert-Butylamine → N-tert-butyl-4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridin-2-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tert-Butylamine | HCID 6385 | — |
| 반응물 | Toluene-p-sulphonic anhydride | HCID 77773 | — |
| 반응물 | 4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridine 1-oxide | HCID 67184479 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | (Trifluoromethyl)benzene | HCID 7368 | — |
| 생성물 | N-tert-butyl-4-[1-(4-methoxybenzyl)-3-(3-nitrophenyl)-1H-pyrazol-4-yl]pyridin-2-amine | HCID 67185904 | 75% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08946250B2 |
| 출처 데이터셋 | uspto-grants-2015_02 |
| ORD ID | ord-9fa05e8f432c4aaaac93fd42ead53fa4 |
| 출처 메모 | uspto-grants-2015_02 |