Amlodipine → HCID 20199195, 화합물

HRID 543137

반응식

HRID 543137 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 20199195HCID 20199195, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-61848bf485f04a79bd5bb6ea400e164c
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04661485

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