Lithium hydroxide, monohydrate → HCID 67248550、化合物

HRID 84277ノート

反応式

HRID 84277 の反応式
[CH3:1][C:2]([S:24]([CH3:27])(=[O:26])=[O:25])([CH2:8][CH2:9][N:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[C:12]([CH3:22])[C:11]1=[O:23])[C:3]([O:5]CC)=[O:4].O.[OH-].[Li+]>O1CCCC1.CO.O.Cl>[CH3:1][C:2]([S:24]([CH3:27])(=[O:25])=[O:26])([CH2:8][CH2:9][N:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)=[C:12]([CH3:22])[C:11]1=[O:23])[C:3]([OH:5])=[O:4]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 67248376ethyl 2-methyl-4-(3-methyl-2-oxo-4-phenylpyridin-1(2H)-yl)-2-(methylsulfonyl)butanoate

生成物 1

HCID 67248550HCID 67248550、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 21892291Methanol tetrahydrofuran water溶媒

実験手順

To a solution of ethyl 2-methyl-4-(3-methyl-2-oxo-4-phenylpyridin-1(2H)-yl)-2-(methylsulfonyl)butanoate (118.3 mg, 0.313 mmol) in tetrahydrofuran/methanol/water (4:1:1, 3.13 mL) was added lithium hydroxide monohydrate (26.3 mg, 0.626 mmol). The mixture was stirred at ambient temperature overnight. The mixture was diluted with aqueous HCl (1N in water) and extracted with ethyl acetate 2×. The combined organic extracts were dried over magnesium sulfate, filtered and concentrated to dryness to afford 2-methyl-4-(3-methyl-2-oxo-4-phenylpyridin-1(2H)-yl)-2-(methylsulfonyl)butanoic acid as a solid. 109.4 mg.

後処理

  1. extractionextracted with ethyl acetate 2×
  2. dry with materialThe combined organic extracts were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-e69696319fd846548b8b238c6be49416
出典データセット
uspto-grants-2014_09
特許番号
US08846933B2

反応ノート

読み込み中…