Dimethylformamide → Methyl 4-[(4-chlorophenyl)sulfanyl]thiophene-3-carboxylate

HRID 1944419노트

반응식

HRID 1944419 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[C:10]([C:14]([OH:16])=[O:15])=[CH:11][S:12][CH:13]=2)=[CH:4][CH:3]=1.[C:17](=O)([O-])O.[Na+].IC.CN(C)C=O>O>[CH3:17][O:15][C:14]([C:10]1[C:9]([S:8][C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)=[CH:13][S:12][CH:11]=1)=[O:16]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 516892Sodium BicarbonateHCID 27789464-[(4-Chlorophenyl)thio]thiophene-3-carboxylic acid

생성물 1

HCID 2778937Methyl 4-[(4-chlorophenyl)sulfanyl]thiophene-3-carboxylate수율 95.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 4-(4-chlorophenylsulfanyl)thiophene-3-carboxylic acid (1.0 g), sodium hydrogen carbonate (1.6 g), iodomethane (2.3 mL) and N,N-dimethylformamide (10 mL) was stirred was stirred at 40° C. for 5 hours. The mixture was cooled to room temperature, diluted with water (100 mL) and the aqueous phase extracted with ethyl acetate. The combined organic extract was dried over magnesium sulfate and concentrated under reduced pressure to afford the title compound as a yellow oil (1.0 g).

후처리

  1. stirringwas stirred at 40° C. for 5 hours
  2. extractionthe aqueous phase extracted with ethyl acetate
  3. extractionThe combined organic extract
  4. dry with materialwas dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8e29b40dcd244a228ebf2768ae96b247
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394836B2

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