Ethylacetate heptane → 6-chloro-N-methyl-4-o-tolylpyridazin-3-amine

HRID 403376

반응식

[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[CH3:15])[CH:3]=1.[CH3:16]CCCCCC.C(OCC)(=O)C>>[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH:8][CH3:16])=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[CH3:15])[CH:3]=1

참가 물질

반응물 2

HCID 21899848Ethylacetate heptane

HCID 866984776-Chloro-4-o-tolylpyridazin-3-ylamine

생성물 1

HCID 866984766-chloro-N-methyl-4-o-tolylpyridazin-3-amine수율 17%

실험 절차

The title compound was prepared in analogy to example 1, intermediate a, from 6-chloro-4-o-tolyl-pyridazin-3-ylamine and using a gradient of n-heptane:ethyl acetate (100:0 to 0:70) eluant for the chromatographic purification. A second purification step on a 20 g column using an MPLC (Flashmaster) system (gradient of n-heptane:ethyl acetate (100:0 to 40:60)) furnished the title compound as a colorless solid (17%). MS (ESI+): m/z=234.080 ([M+H]+).

후처리

customfor the chromatographic purification
customA second purification step on a 20 g column

출처 및 근거

ORD 기록: ord-10f9c93005484fd3b931f020b563f171
출처 데이터셋: uspto-grants-2014_06
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08748434B2

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