Lithium hydroxide, monohydrate → 6-{2-[2-(4-Chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-acetylamino}-nicotinic acid

HRID 1161344ノート

反応式

HRID 1161344 の反応式
C[O:2][C:3](=[O:38])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11](=[O:37])[CH:12]([N:19]2[C:23]3[CH:24]=[C:25]([F:29])[C:26]([F:28])=[CH:27][C:22]=3[N:21]=[C:20]2[C:30]2[CH:35]=[CH:34][C:33]([Cl:36])=[CH:32][CH:31]=2)[CH:13]2[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]2)=[N:6][CH:5]=1.O.[OH-].[Li+]>O.O1CCOCC1>[Cl:36][C:33]1[CH:34]=[CH:35][C:30]([C:20]2[N:19]([CH:12]([CH:13]3[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]3)[C:11]([NH:10][C:7]3[CH:8]=[CH:9][C:4]([C:3]([OH:38])=[O:2])=[CH:5][N:6]=3)=[O:37])[C:23]3[CH:24]=[C:25]([F:29])[C:26]([F:28])=[CH:27][C:22]=3[N:21]=2)=[CH:31][CH:32]=1

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 686452646-{2-[2-(4-Chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-acetylamino}-nicotinic acid methyl ester

生成物 1

HCID 441987326-{2-[2-(4-Chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-acetylamino}-nicotinic acid収率 95.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

6-{2-[2-(4-Chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-acetylamino}-nicotinic acid methyl ester (24 mg, 0.04 mmol) was dissolved in water (0.5 ml) and dioxane (0.5 ml). Lithium hydroxide monohydrate (9 eq, 17 mg) was added and the mixture stirred 3 h at room temperature. The dioxane was removed under reduced pressure and the residue acidified to pH2 with 3M aqueous hydrochloric acid. The precipitate was filtered to afford the title compound as a white solid (20 mg, 84%).

後処理

  1. customThe dioxane was removed under reduced pressure
  2. filtrationThe precipitate was filtered

出典と根拠

ORDレコード
ord-6cac8ab46fe547d0bd486a018cb8fb74
出典データセット
uspto-grants-2010_10
特許番号
US07816540B2

反応ノート

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