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

HRID 1003316노트

반응식

HRID 1003316 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9f1225e7359d460ea87081127b400aa0
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06046201

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