Hydrochloric Acid → HCID 20074046, 화합물

HRID 704444노트

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HRID 704444 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:11]2[NH:15][CH:14]([C:16]([N:18]3[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][CH2:26][C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[CH2:20][CH2:19]3)=[O:17])[CH2:13][S:12]2)[CH:6]=[N:7][C:8]=1[O:9]C.Cl>C(OCC)(=O)C.O1CCOCC1>[CH3:1][O:2][CH:3]1[C:8](=[O:9])[N:7]=[CH:6][C:5]([CH:11]2[NH:15][CH:14]([C:16]([N:18]3[CH2:19][CH2:20][N:21]([CH2:24][CH2:25][CH2:26][C:27]4[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=4)[CH2:22][CH2:23]3)=[O:17])[CH2:13][S:12]2)=[CH:4]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 14881563HCID 14881563, 화합물

생성물 1

HCID 20074046HCID 20074046, 화합물수율 29.7%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

1-[2-(5,6-Dimethoxy-3-pyridyl)thiazolidin-4-ylcarbonyl]-4-(3-phenylpropyl)piperazine (730 mg) was dissolved in 25 ml of ethyl acetate. To the solution was added with stirring at room temperature 2N hydrogen chloride solution in dioxane. The resultant powder was collected by filtration and dissolved in saturated sodium carbonate solution. Ethyl acetate was added, the organic layer was separated and washed with water, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (silica gel 25 ml; 10% methanol-ethyl acetate) to give 210 mg of 1-[2-(5-methoxy-6 oxo 5,6-dihydro-3-pyridyl)thiazolidin-4-ylcarbonyl]-4-(3-phenylpropyl)piperazine.

후처리

  1. additionTo the solution was added
  2. filtrationThe resultant powder was collected by filtration
  3. dissolutiondissolved in saturated sodium carbonate solution
  4. additionEthyl acetate was added
  5. customthe organic layer was separated
  6. washwashed with water
  7. distillationthe solvent was distilled off under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (silica gel 25 ml; 10% methanol-ethyl acetate)

출처 및 근거

ORD 기록
ord-0e48d80a79d2402485676bd68e71082c
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04987132

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