Toluene → HCID 86588863、化合物

HRID 1790194ノート

反応式

HRID 1790194 の反応式
C1(C)C=CC=CC=1.N1CCCCC1.[CH3:14][N:15]1[C:24]2[C:19](=[CH:20][C:21]([CH3:38])=[C:22]([C:25]3[CH:26]=[C:27]([CH:30]=[CH:31][C:32]=3[O:33][C:34]([F:37])([F:36])[F:35])[CH:28]=O)[CH:23]=2)[C:18]([CH3:40])([CH3:39])[CH2:17][C:16]1=[O:41].[CH3:42][N:43]1[C:47](=[O:48])[CH2:46][S:45][C:44]1=[O:49]>C(OCC)(=O)C.C(O)(=O)C>[CH3:42][N:43]1[C:47](=[O:48])[C:46](=[CH:28][C:27]2[CH:30]=[CH:31][C:32]([O:33][C:34]([F:37])([F:36])[F:35])=[C:25]([C:22]3[CH:23]=[C:24]4[C:19]([C:18]([CH3:39])([CH3:40])[CH2:17][C:16](=[O:41])[N:15]4[CH3:14])=[CH:20][C:21]=3[CH3:38])[CH:26]=2)[S:45][C:44]1=[O:49]

参加物

7

反応物 4

HCID 1140TolueneHCID 8082PiperidineHCID 12820623-Methyl-1,3-thiazolidine-2,4-dioneHCID 21966438HCID 21966438、化合物

生成物 1

HCID 86588863HCID 86588863、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of toluene (80 mL), piperidine (380 μL), acetic acid (380 μL), 3-(1,4,4,6-Tetramethyl-2-oxo-1,2,3,4-tetrahydro-quinolin-7-yl)-4-trifluoromethoxy-benzaldehyde (7.5 g, 19.16 mmol) and a 3-alkyl—thiazolidine-2,4-dione such as 3-Methyl-thiazolidine-2,4-dione (19.16 mmol) is heated at reflux overnight. The reaction mixture is cooled to room temperature, diluted with ethyl acetate and is washed with water and brine, dried over MgSO4. The residue is recrystallized to afford 3-methyl-5-[3-(1,4,4,6-tetramethyl-2-oxo-1,2,3,4-tetrahydro-quinolin-7-yl)-4-trifluoromethoxy-benzylidene]-thiazolidine-2,4-dione.

後処理

  1. temperatureat reflux overnight
  2. washis washed with water and brine
  3. dry with materialdried over MgSO4
  4. customThe residue is recrystallized

出典と根拠

ORDレコード
ord-5b00ee9768ad48a898dd923a0cb62874
出典データセット
uspto-grants-2006_07
特許番号
US07071218B2

反応ノート

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