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

HRID 403376

反応式

HRID 403376 の反応式
[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

参加物

3

反応物 2

HCID 21899848Ethylacetate heptaneHCID 866984776-Chloro-4-o-tolylpyridazin-3-ylamine

生成物 1

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

実験手順

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]+).

後処理

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

出典と根拠

ORDレコード
ord-10f9c93005484fd3b931f020b563f171
出典データセット
uspto-grants-2014_06
特許番号
US08748434B2

関連ノート

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