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

HRID 1602935노트

반응식

HRID 1602935 반응식
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]

참가 물질

6

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f22d7c889e74403c910ba11a563cf17e
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05985894

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