Hydrazine hydrate (1:1) → Dimethyl 4-[2-(4-aminobutoxy)-5-methylsulfonylphenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate

HRID 4659ノート

反応式

HRID 4659 の反応式
C1(=O)[N:5]([CH2:6][CH2:7][CH2:8][CH2:9][O:10][C:11]2[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:19])=[O:18])=[CH:13][C:12]=2[CH:21]2[C:26]([C:27]([O:29][CH3:30])=[O:28])=[C:25]([CH3:31])[NH:24][C:23]([CH3:32])=[C:22]2[C:33]([O:35][CH3:36])=[O:34])C(=O)C2=CC=CC=C12.O.NN>C(O)C>[NH2:5][CH2:6][CH2:7][CH2:8][CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:18])=[O:19])=[CH:13][C:12]=1[CH:21]1[C:26]([C:27]([O:29][CH3:30])=[O:28])=[C:25]([CH3:31])[NH:24][C:23]([CH3:32])=[C:22]1[C:33]([O:35][CH3:36])=[O:34]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 20151519Dimethyl 4-[2-(4-phthalimidobutoxy)-5-methylsulfonylphenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate

生成物 1

HCID 14050493Dimethyl 4-[2-(4-aminobutoxy)-5-methylsulfonylphenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate収率 48.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 6.9 g of dimethyl 4-[2-(4-phthalimidobutoxy)-5-methylsulfonylphenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate and 5.9 g of hydrazine monohydrate in 170 ml of % ethanol(water: 5%) was refluxed under heating for 6 hours. After cooling, the reaction solution was concentrated under reduced pressure. The residue was extracted with chloroform, and the extract was washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. Crude crystals thus obtained were recrystallized from chloroform-ether to give 2.6 g of dimethyl 4-[2-(4-aminobutoxy)-5-methylsulfonylphenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate.

後処理

  1. temperatureunder heating for 6 hours
  2. temperatureAfter cooling
  3. concentrationthe reaction solution was concentrated under reduced pressure
  4. extractionThe residue was extracted with chloroform
  5. washthe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customCrude crystals thus obtained
  9. customwere recrystallized from chloroform-ether

出典と根拠

ORDレコード
ord-3665349bb73843b2bd458f0e58887d4d
出典データセット
uspto-grants-1988_02
特許番号
US04727082

反応ノート

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