Water → 3-chloro-4-(N-(4-chlorobenzenesulphonyl)-N-methylaminomethyl)thiophene-2-carboxylic acid

HRID 901955

反応式

HRID 901955 の反応式
[OH-].[Li+].O.[Cl:4][C:5]1[C:9]([CH2:10][N:11]([S:13]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)(=[O:15])=[O:14])[CH3:12])=[CH:8][S:7][C:6]=1[C:23]([O:25]C)=[O:24]>O1CCOCC1>[Cl:4][C:5]1[C:9]([CH2:10][N:11]([S:13]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=2)(=[O:15])=[O:14])[CH3:12])=[CH:8][S:7][C:6]=1[C:23]([OH:25])=[O:24]

参加物

5

反応物 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 69208322methyl 3-chloro(N-(4-chlorobenzenesulphonyl)-N-methylaminomethyl)thiophene-2-carboxylate

生成物 1

HCID 692074073-chloro-4-(N-(4-chlorobenzenesulphonyl)-N-methylaminomethyl)thiophene-2-carboxylic acid収率 84.2%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Lithium hydroxide (210 mg, 5.0 mmol) and water (10 ml) were added to a solution of methyl 3-chloro-4-(N-(4-chlorobenzenesulphonyl)-N-methylaminomethyl)thiophene-2-carboxylate (990 mg, 2.5 mmol) in dioxan (20 ml) and the mixture stirred for 18 h. The mixture was evaporated and 0.3N potassium hydrogen sulphate was added. The mixture was extracted with ethyl acetate and the organic extracts were washed with water and brine, dried and reduced to afford 3-chloro-4-(N-(4-chlorobenzenesulphonyl)-N-methylaminomethyl)thiophene-2-carboxylic acid (800 mg, 84%) as a white solid.

後処理

  1. customThe mixture was evaporated
  2. addition0.3N potassium hydrogen sulphate was added
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe organic extracts were washed with water and brine
  5. customdried

出典と根拠

ORDレコード
ord-71aa40e6c4c14ecbaeb8ed96d5082c6c
出典データセット
uspto-grants-2008_04
特許番号
US07365065B2

関連ノート

読み込み中…