Amlodipine → HCID 20199195、化合物

HRID 543137

反応式

HRID 543137 の反応式
[NH2:1][CH2:2][CH2:3][O:4][CH2:5][C:6]1[NH:7][C:8]([CH3:28])=[C:9]([C:24]([O:26][CH3:27])=[O:25])[CH:10]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:23])[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13].CS[C:31]1[NH:36][C:35](=[O:37])[CH:34]=[CH:33][N:32]=1>C(O)C>[Cl:23][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[CH:10]1[C:9]([C:24]([O:26][CH3:27])=[O:25])=[C:8]([CH3:28])[NH:7][C:6]([CH2:5][O:4][CH2:3][CH2:2][NH:1][C:31]2[NH:36][C:35](=[O:37])[CH:34]=[CH:33][N:32]=2)=[C:11]1[C:12]([O:14][CH2:15][CH3:16])=[O:13]

参加物

4

反応物 2

HCID 2162AmlodipineHCID 798232-(Methylthio)-1H-pyrimidin-4-one

生成物 1

HCID 20199195HCID 20199195、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-[2-Aminoethoxymethyl]-3-ethoxycarbonyl-4-(2-chlorophenyl)-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine (0.75 g) and 2-methylthio-3H-pyrimid-4-one (0.5 g) were dissolved in ethanol (5 ml) and heated under reflux for 20 hours. The solvent was evaporated and the residue was partitioned between ethyl acetate and water. The organic layer was separated, washed with 2N hydrochloric acid to remove any unreacted amine, and then with dilute sodium hydroxide solution. It was then washed with water, dried, filtered and evaporated to give a yellow gum. Chromatography on silica "Kieselgel 60H" (Trade Mark) eluting with ethyl acetate gave the title compound, which was recrystallised from ethyl acetate, yield 171 mg, m.p. 148°-150°.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 20 hours
  3. customThe solvent was evaporated
  4. customthe residue was partitioned between ethyl acetate and water
  5. customThe organic layer was separated
  6. washwashed with 2N hydrochloric acid
  7. customto remove any unreacted amine
  8. washIt was then washed with water
  9. customdried
  10. filtrationfiltered
  11. customevaporated
  12. customto give a yellow gum
  13. washChromatography on silica "Kieselgel 60H" (Trade Mark) eluting with ethyl acetate

出典と根拠

ORDレコード
ord-61848bf485f04a79bd5bb6ea400e164c
出典データセット
uspto-grants-1987_04
特許番号
US04661485

関連ノート

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