Water → HCID 19962365、化合物

HRID 53334ノート

反応式

HRID 53334 の反応式
[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

参加物

5

反応物 3

HCID 962WaterHCID 11430Potassium Carbonate2 回HCID 199623683-[2-[(4-Chlorophenyl)sulphonylamino]ethyl]-5-(4-fluorobenzoyl)benzenepropanoic acid

生成物 1

HCID 19962365HCID 19962365、化合物収率 85.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-124031ecb21442b89a16ecd519315e68
出典データセット
uspto-grants-1997_04
特許番号
US05618941

反応ノート

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