Hydrazine hydrate (1:1) → 5-{[4-(2-Chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxymethyl}-3-pyrazolone

HRID 1589148ノート

反応式

HRID 1589148 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[C:13]([C:14]([O:16][CH3:17])=[O:15])=[C:12]([CH3:18])[NH:11][C:10]([CH2:19][O:20][CH2:21][C:22](=O)[CH2:23][C:24]([O:26]CC)=O)=[C:9]1[C:30]([O:32][CH2:33][CH3:34])=[O:31].O.[NH2:36][NH2:37]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[C:13]([C:14]([O:16][CH3:17])=[O:15])=[C:12]([CH3:18])[NH:11][C:10]([CH2:19][O:20][CH2:21][C:22]2[N:37]=[N:36][C:24](=[O:26])[CH:23]=2)=[C:9]1[C:30]([O:32][CH2:33][CH3:34])=[O:31]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 70044209Ethyl 4-{[4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxy}acetoacetate

生成物 1

HCID 202481365-{[4-(2-Chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxymethyl}-3-pyrazolone収率 38.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of ethyl 4-{[4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-1,4-dihydropyridin-2-yl]methoxy}acetoacetate (0.50 g) and hydrazine hydrate (0.50 g) in ethanol (20 ml) was kept at room temperature for 4 days and then evaporated. The residue was purified by chromatography on silica gel (1.0 g) using dichloromethane plus 0-5% by volume of methanol as eluant. Appropriate fractions were combined and evaporated and the residue crystallised from ethyl acetate to give the title compound (0.18 g), m.p. 207° C. Found: C,57.11; H,5.15; N,9.19. C22H24ClN3O6 requires: C,57.20; H,5.24; N,9.10%.

後処理

  1. customevaporated
  2. customThe residue was purified by chromatography on silica gel (1.0 g)
  3. customevaporated
  4. customthe residue crystallised from ethyl acetate

出典と根拠

ORDレコード
ord-a50ddc7333e64d9d8dbf893a25f4030f
出典データセット
uspto-grants-1986_02
特許番号
US04568677

反応ノート

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