Hydrochloric Acid → HCID 20074046、化合物

HRID 704444ノート

反応式

HRID 704444 の反応式
[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

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 14881563HCID 14881563、化合物

生成物 1

HCID 20074046HCID 20074046、化合物収率 29.7%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-0e48d80a79d2402485676bd68e71082c
出典データセット
uspto-grants-1991_01
特許番号
US04987132

反応ノート

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