3-(Morpholine-4-sulfonyl)-5-trifluoromethyl-benzoic acid → HCID 71766225、化合物

HRID 403381ノート

反応式

HRID 403381 の反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH:8][CH3:9])=[C:4]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:3]=1.N1([S:22]([C:25]2[CH:26]=[C:27]([CH:31]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:33]=2)[C:28]([OH:30])=O)(=[O:24])=[O:23])CCOCC1.[CH3:38]CCCCCC.C(OCC)(=O)C>>[Cl:1][C:2]1[N:7]=[N:6][C:5]([N:8]([CH3:9])[C:28](=[O:30])[C:27]2[CH:31]=[C:32]([C:34]([F:35])([F:36])[F:37])[CH:33]=[C:25]([S:22]([CH3:38])(=[O:23])=[O:24])[CH:26]=2)=[C:4]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:3]=1

参加物

4

反応物 3

HCID 179642763-(Morpholine-4-sulfonyl)-5-trifluoromethyl-benzoic acidHCID 21899848Ethylacetate heptaneHCID 866984786-chloro-N-methyl-4-phenylpyridazin-3-amine

生成物 1

HCID 71766225HCID 71766225、化合物収率 14%

実験手順

The title compound was prepared in analogy to example 1, from (6-chloro-4-phenyl-pyridazin-3-yl)-methyl-amine (example 5, intermediate a) and 3-(morpholine-4-sulfonyl)-5-trifluoromethyl-benzoic acid and using a gradient of n-heptane:ethyl acetate (100:0 to 30:70) for the chromatographic purification. Another purification step using preparative HPLC (Gemini NX column) with a gradient of methanol:water with 0.05% formic acid (80:20 to 98:2) furnished the title compound as a colorless solid (14%). MS (ESI+): m/z=541.090 ([M+H]+).

後処理

  1. customfor the chromatographic purification
  2. customAnother purification step

出典と根拠

ORDレコード
ord-7c22745da4754cd997e023aecb40fb4f
出典データセット
uspto-grants-2014_06
特許番号
US08748434B2

反応ノート

読み込み中…