Methylhydrazine → 3-Isopropyl-1-methyl-1H-pyrazol-5-amine

반응식

[CH3:1][CH:2]([CH3:9])[C:3](=C=O)[CH2:4][C:5]#[N:6].[CH3:10][NH:11][NH2:12]>>[CH3:10][N:11]1[C:5]([NH2:6])=[CH:4][C:3]([CH:2]([CH3:1])[CH3:9])=[N:12]1

참가 물질

반응물 2

HCID 6061Methylhydrazine

HCID 866857984-Methyl-3-carbonyl valeronitrile

생성물 1

HCID 27594993-Isopropyl-1-methyl-1H-pyrazol-5-amine수율 51.9%

실험 절차

Under nitrogen atmosphere, the compound of Example 2A (8.03 g, 72 mmol) was dissolved in alcohol (50 mL). Methylhydrazine (3.32 g, 72 mmol) was added. The resultant mixture was slowly warmed and refluxed with stirring. The reaction was kept for 3 hr. The reaction was stopped and cooled to room temperature. Alcohol was rotary-evaporated to obtain a crude product as oil. The crude product was purified with column chromatography (eluant: petroleum ether/ethyl acetate=1:1) to give 5.2 g of the title compound. MS (ESI): m/z 140 (M+H)+

후처리

temperaturerefluxed
customAlcohol was rotary-evaporated
customto obtain a crude product as oil
customThe crude product was purified with column chromatography (eluant: petroleum ether/ethyl acetate=1:1)

출처 및 근거

ORD 기록: ord-b0a427dbb42b4f299a59db135276713d
출처 데이터셋: uspto-grants-2016_02
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09249172B2

반응 노트

불러오는 중…