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

HRID 901955

반응식

HRID 901955 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-71aa40e6c4c14ecbaeb8ed96d5082c6c
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07365065B2

연결된 노트

불러오는 중…