Sodium Methoxide → HCID 89691264、化合物

HRID 2203091ノート

反応式

HRID 2203091 の反応式
Cl.[CH:2]1([C:5]2[N:9]([CH3:10])[C:8]3[CH:11]=[C:12]([N:15]4[CH:20]=[CH:19][C:18]([O:21][CH2:22][C:23](=[NH:25])[NH2:24])=[CH:17][C:16]4=[O:26])[CH:13]=[CH:14][C:7]=3[N:6]=2)[CH2:4][CH2:3]1.F[P-](F)(F)(F)(F)F.[Cl:34][C:35](=[CH:40]N(C)C)[CH:36]=[N+](C)C.C[O-].[Na+]>CO>[Cl:34][C:35]1[CH:36]=[N:25][C:23]([CH2:22][O:21][C:18]2[CH:19]=[CH:20][N:15]([C:12]3[CH:13]=[CH:14][C:7]4[N:6]=[C:5]([CH:2]5[CH2:4][CH2:3]5)[N:9]([CH3:10])[C:8]=4[CH:11]=3)[C:16](=[O:26])[CH:17]=2)=[N:24][CH:40]=1

参加物

5

反応物 3

HCID 10942334Sodium MethoxideHCID 748906302-Chloro-3-(dimethylamino)-N,N-dimethylprop-2-en-1-iminium hexafluoridophosphate(1-)HCID 89691033HCID 89691033、化合物

生成物 1

HCID 89691264HCID 89691264、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2-((1-(2-cyclopropyl-1-methyl-1H-benzimidazol-6-yl)-2-oxo-1,2-dihydropyridin-4-yl)oxy)ethanimidamide hydrochloride (100 mg), 2-chloro-3-(dimethylamino)-N,N-dimethylprop-2-en-1-iminium hexafluorophosphate (0.82 ml), sodium methoxide (43.3 mg) and MeOH (10 ml) was stirred at room temperature for 1 h. The mixture was concentrated, and the residue was partitioned between EtOAc and water. The extract was washed with brine, dried over MgSO4, concentrated and purified by NH silica gel column chromatography (hexane/EtOAc) to give the title compound (56 mg) as a white solid.

後処理

  1. concentrationThe mixture was concentrated
  2. customthe residue was partitioned between EtOAc and water
  3. washThe extract was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. custompurified by NH silica gel column chromatography (hexane/EtOAc)

出典と根拠

ORDレコード
ord-64f982d5672947d69216678564675f89
出典データセット
uspto-grants-2016_06
特許番号
US09365540B2

反応ノート

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