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Potassium Carbonate → N-(2,3-dihydro-2,2-dimethylbenzofuran-7-yl)sulfonyl-2-[2-chloro-4-fluoro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]propionamide

HRID 1252343
ノート
印刷プレビュー

反応式

HRID 1252343 の反応式
[Cl:1][C:2]1[C:7]([OH:8])=[CH:6][C:5]([N:9]2[C:13](=[O:14])[N:12]([CH:15]([F:17])[F:16])[C:11]([CH3:18])=[N:10]2)=[C:4]([F:19])[CH:3]=1.[CH3:20][C:21]1([CH3:39])[CH2:25][C:24]2[CH:26]=[CH:27][CH:28]=[C:29]([S:30]([NH:33][C:34](=[O:38])[CH:35](Br)[CH3:36])(=[O:32])=[O:31])[C:23]=2[O:22]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:39][C:21]1([CH3:20])[CH2:25][C:24]2[CH:26]=[CH:27][CH:28]=[C:29]([S:30]([NH:33][C:34](=[O:38])[CH:35]([O:8][C:7]3[CH:6]=[C:5]([N:9]4[C:13](=[O:14])[N:12]([CH:15]([F:16])[F:17])[C:11]([CH3:18])=[N:10]4)[C:4]([F:19])=[CH:3][C:2]=3[Cl:1])[CH3:36])(=[O:32])=[O:31])[C:23]=2[O:22]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 137694562-(4-Chloro-2-fluoro-5-hydroxyphenyl)-4-(difluoromethyl)-5-methyl-2,4-dihydro-3H-1,2,4-triazol-3-oneHCID 15611040N-(2,3-dihydro-2,2-dimethylbenzofuran-7-yl)sulfonyl-2-bromopropionamide

生成物 1

HCID 15611068N-(2,3-dihydro-2,2-dimethylbenzofuran-7-yl)sulfonyl-2-[2-chloro-4-fluoro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]propionamide

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A stirred mixture of 0.2 gram (0.0007 mole) of 1-(4-chloro-2-fluoro-5-hydroxyphenyl)-4-difluoromethyl-4,5-dihydro-3-methyl-1,2,4-triazol-5(1H)-one, 0.3 gram (0.0007 mole) of N-(2,3-dihydro-2,2-dimethylbenzofuran-7-yl)sulfonyl-2-bromopropionamide, 0.3 gram (0.002 mole) of potassium carbonate in 20 ml of acetone was heated under reflux for 18 hours. The reaction mixture was cooled and concentrated under reduced pressure to a residue. The residue was dissolved in 100 ml of water and the solution acidified by the dropwise addition of concentrated hydrochloric acid. The resultant precipitate was collected by filtration, washed with water, and dried to yield N-(2,3-dihydro-2,2-dimethylbenzofuran-7-yl)sulfonyl-2-[2-chloro-4-fluoro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]propionamide; m.p. 198°-201° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. temperatureThe reaction mixture was cooled
  4. concentrationconcentrated under reduced pressure to a residue
  5. dissolutionThe residue was dissolved in 100 ml of water
  6. additionthe solution acidified by the dropwise addition of concentrated hydrochloric acid
  7. filtrationThe resultant precipitate was collected by filtration
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-f23b655503864a0c921a7bc857d3738d
出典データセット
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04743291

反応ノート

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