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Sulfuric Acid → 3-(2,2-Diethoxyethyl)amino-2-methyl-4-(methylsulfonyl)benzoic acid

HRID 547249
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HRID 547249 반응식
F[C:2]1[C:3]([CH3:15])=[C:4]([CH:8]=[CH:9][C:10]=1[S:11]([CH3:14])(=[O:13])=[O:12])[C:5]([OH:7])=[O:6].[CH2:16]([O:18][CH:19]([O:22][CH2:23][CH3:24])[CH2:20][NH2:21])[CH3:17].OS(O)(=O)=O>>[CH2:16]([O:18][CH:19]([O:22][CH2:23][CH3:24])[CH2:20][NH:21][C:2]1[C:3]([CH3:15])=[C:4]([CH:8]=[CH:9][C:10]=1[S:11]([CH3:14])(=[O:13])=[O:12])[C:5]([OH:7])=[O:6])[CH3:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 695242,2-DiethoxyethylamineHCID 142544793-Fluoro-2-methyl-4-(methylsulfonyl)benzoic acid

생성물 1

HCID 671984093-(2,2-Diethoxyethyl)amino-2-methyl-4-(methylsulfonyl)benzoic acid

반응 조건

온도
120 °C

실험 절차

5.1 g (22 mmol) of 3-fluoro-2-methyl-4-(methylsulfonyl)benzoic acid were dissolved in 30 ml (218 mmol) of aminoacetaldehyde diethyl acetal. The mixture was heated at 120° C. with stirring for 2 days, cooled to RT, acidified with 10% strength H2SO4 and extracted twice with ethyl acetate. The combined organic phases were dried over MgSO4, and the solvent was removed under reduced pressure. This gave 4.0 g of a yellow oil of a purity of 91%.

후처리

  1. temperaturecooled to RT
  2. extractionextracted twice with ethyl acetate
  3. dry with materialThe combined organic phases were dried over MgSO4
  4. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-89690ad9344d42e9a88f58b1e6e6c7a6
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07939467B2

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