Water → HCID 19962365, 화합물

HRID 53334노트

반응식

HRID 53334 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][CH2:12][CH2:13][C:14]2[CH:15]=[C:16]([CH2:29][CH2:30][C:31]([OH:33])=[O:32])[CH:17]=[C:18]([C:20](=[O:28])[C:21]3[CH:26]=[CH:25][C:24](F)=[CH:23][CH:22]=3)[CH:19]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[C:34](=O)([O-])[O-:35].[K+].[K+].O>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][CH2:12][CH2:13][C:14]2[CH:15]=[C:16]([CH2:29][CH2:30][C:31]([OH:33])=[O:32])[CH:17]=[C:18]([C:20](=[O:28])[C:21]3[CH:26]=[CH:25][C:24]([O:35][CH3:34])=[CH:23][CH:22]=3)[CH:19]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 11430Potassium Carbonate2회HCID 199623683-[2-[(4-Chlorophenyl)sulphonylamino]ethyl]-5-(4-fluorobenzoyl)benzenepropanoic acid

생성물 1

HCID 19962365HCID 19962365, 화합물수율 85.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 3-[2-[(4-chlorophenyl)sulphonylamino]ethyl]-5-(4-fluorobenzoyl)benzenepropanoic acid (0.25 g) and potassium carbonate (0.212 g) in anhydrous methanol (5.0 ml) was heated under reflux for 18 hours. Additional potassium carbonate (0.212 g) was added and the mixture was heated under reflux for a further 20 hours and then cooled. Water (15 ml) was added and the solution was evaporated to about 10 ml and then acidified with 2N hydrochloric acid. The mixture was extracted several times with ethyl acetate and the combined extracts were washed with water and dried (MgSO4). Evaporation of the solvent gave the title compound as a glass (0.22 g). Found: C,60.25; H,4.92; N,2.51. C25H24ClNO6S requires C,59.81; H,4.82; N,2.79%.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. temperaturethe mixture was heated
  4. temperatureunder reflux for a further 20 hours
  5. temperaturecooled
  6. customthe solution was evaporated to about 10 ml
  7. extractionThe mixture was extracted several times with ethyl acetate
  8. washthe combined extracts were washed with water
  9. dry with materialdried (MgSO4)
  10. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-124031ecb21442b89a16ecd519315e68
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05618941

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