Methanol → Sodium 6-(4-ethylpiperazinyl)pyridine-3-carboxylate

HRID 1003316ノート

反応式

HRID 1003316 の反応式
[OH-].[Na+:2].CO.[CH2:5]([N:7]1[CH2:12][CH2:11][N:10]([C:13]2[N:18]=[CH:17][C:16]([C:19]([O:21]C)=[O:20])=[CH:15][CH:14]=2)[CH2:9][CH2:8]1)[CH3:6]>O>[CH2:5]([N:7]1[CH2:8][CH2:9][N:10]([C:13]2[N:18]=[CH:17][C:16]([C:19]([O-:21])=[O:20])=[CH:15][CH:14]=2)[CH2:11][CH2:12]1)[CH3:6].[Na+:2]

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 14987929Methyl 6-(4-ethylpiperazin-1-yl)nicotinate

生成物 1

HCID 23663821Sodium 6-(4-ethylpiperazinyl)pyridine-3-carboxylate収率 111.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 3.1 g of sodium hydroxide in 15 ml of water was added to 75 ml of methanol. 15 g of methyl 6-(4-ethyl-1-piperazinyl)pyridine-3-carboxylate was added and the mixture was heated under reflux for 1.5 hours. The solvent was distilled off under reduced pressure, to the resulting residue was added hot acetone and the crystal thus precipitated out was recovered by filtration. It was again washed with hot acetone to afford 17.2 g of the title compound as a crystal.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. distillationThe solvent was distilled off under reduced pressure, to the resulting residue
  4. additionwas added hot acetone
  5. customthe crystal thus precipitated out
  6. filtrationwas recovered by filtration
  7. washIt was again washed with hot acetone

出典と根拠

ORDレコード
ord-9f1225e7359d460ea87081127b400aa0
出典データセット
uspto-grants-2000_04
特許番号
US06046201

反応ノート

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