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Sodium Hydroxide → HCID 14052179, 화합물

HRID 1030796
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HRID 1030796 반응식
[OH-].[Na+].[SH:3][C:4]1[C:13]([CH3:14])=[N:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1.Cl.[CH2:16]([N:18]([CH2:27][CH3:28])[C:19]1[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=1[CH2:21]Cl)[CH3:17]>O.C(O)C>[CH2:27]([N:18]([CH2:16][CH3:17])[C:19]1[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=1[CH2:21][S:3][C:4]1[C:13]([CH3:14])=[N:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1)[CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 14839433HCID 14839433, 화합물HCID 1784186273-Methylquinoxaline-2-thiol

생성물 1

HCID 14052179HCID 14052179, 화합물수율 60.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a solution of 0.73 g of sodium hydroxide in a mixture of 2 ml of water and 50 ml of ethanol were added successively 1.5 g of 2-mercapto-3-methylquinoxaline and 1.99 g of 2-diethylaminobenzyl chloride hydrochloride. The resulting mixture was stirred at room temperature for 3 hrs., and the solvent was removed under reduced pressure. The residue was extracted with ethyl acetate. The organic layer was washed successively with 5% aqueous sodium hydroxide solution, water and saturated aqueous sodium chloride solution, and then dried over sodium sulfate. The sodium sulfate was removed by filtration, and the filtrate was placed under reduced pressure to remove the solvent. The residual oil was purified by silica gel column chromatography (hexane/acetone) to give 1.74 g of 2-(2-diethylaminobenzylthio)-3-methylquinoxaline as a yellow oil.

후처리

  1. custom, and the solvent was removed under reduced pressure
  2. extractionThe residue was extracted with ethyl acetate
  3. washThe organic layer was washed successively with 5% aqueous sodium hydroxide solution, water and saturated aqueous sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customThe sodium sulfate was removed by filtration
  6. customto remove the solvent
  7. customThe residual oil was purified by silica gel column chromatography (hexane/acetone)

출처 및 근거

ORD 기록
ord-58d8f68a37f14ddebf6ed2e986b8ac40
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05106976

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