Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 3-tert-Butyl-1-(3,4-dimethylphenyl)-1H-pyrazol-5-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Pentanenitrile, 4,4-dimethyl-3-oxo- | HCID 108871 | — |
| 반응물 | 1-(3,4-Dimethylphenyl)hydrazine hydrochloride | HCID 173740 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 3-tert-Butyl-1-(3,4-dimethylphenyl)-1H-pyrazol-5-amine | HCID 10868500 | 66.9% |
반응 단계
To a solution of pivaloylacetonitrile (400 mg) in toluene (10 mL) were added 3,4-dimethylphenylhydrazine hydrochloride (520 mg) and triethylamine (0.4 mL) and refluxed with heating for 5 hours. The reaction mixture was added with a saturated sodium hydrogen carbonate aqueous solution. The obtained organic layer was washed with a saturated sodium chloride aqueous solution. The obtained organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The obtained residue was purified on silica gel column chromatography (hexane:ethyl acetate=4:1) to give the titled compound (490 mg) having the following physical data.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09242977B2 |
| 출처 데이터셋 | uspto-grants-2016_01 |
| ORD ID | ord-c103ebe0bf7f4f7eb4213ff3e0bbd809 |
| 출처 메모 | uspto-grants-2016_01 |