Water → Methyl 4'-[(3-butyl-1,4-dihydro-4-thioxo-1-quinolinyl)-methyl](1,1'-biphenyl)-2-carboxylate

HRID 1602935ノート

反応式

HRID 1602935 の反応式
COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:10])=CC=1.[CH2:23]([C:27]1[C:36](=O)[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[N:29]([CH2:38][C:39]2[CH:44]=[CH:43][C:42]([C:45]3[C:46]([C:51]([O:53][CH3:54])=[O:52])=[CH:47][CH:48]=[CH:49][CH:50]=3)=[CH:41][CH:40]=2)[CH:28]=1)[CH2:24][CH2:25][CH3:26].O.C(OCC)(=O)C>C1(C)C=CC=CC=1>[CH2:23]([C:27]1[C:36](=[S:10])[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[N:29]([CH2:38][C:39]2[CH:44]=[CH:43][C:42]([C:45]3[C:46]([C:51]([O:53][CH3:54])=[O:52])=[CH:47][CH:48]=[CH:49][CH:50]=3)=[CH:41][CH:40]=2)[CH:28]=1)[CH2:24][CH2:25][CH3:26]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 87949Lawesson's reagentHCID 19608515Methyl 4'-[(3-butyl-1,4-dihydro-4-oxo-1-quinolinyl)-methyl](1,1'-biphenyl)-2-carboxylate

生成物 1

HCID 19608518Methyl 4'-[(3-butyl-1,4-dihydro-4-thioxo-1-quinolinyl)-methyl](1,1'-biphenyl)-2-carboxylate収率 26,169.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

2.10 mg of Lawesson reagent were added to a solution of 400 mg of the product of Example 3 in 20 ml of toluene and the mixture was refluxed for 90 minutes. The mixture was poured into 100 ml of water and extraction was carried out with ethyl acetate. Th extracts were washed with water, dried, filtered and evaporated to dryness to obtain 0.6 g of the expected product which was chromatographed on silica (eluant: methylene chloride-acetone (98-2)) to collect 0.42 g of the desired product melting at 158° C.

後処理

  1. temperaturethe mixture was refluxed for 90 minutes
  2. washTh extracts were washed with water
  3. customdried
  4. filtrationfiltered
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-f22d7c889e74403c910ba11a563cf17e
出典データセット
uspto-grants-1999_11
特許番号
US05985894

反応ノート

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