Potassium Carbonate → HCID 14052175, 화합물

HRID 1030787노트

반응식

HRID 1030787 반응식
[SH:1][C:2]1[C:11]([CH3:12])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.Cl.[N:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[CH2:20][Cl:21].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.O>[ClH:21].[CH3:12][C:11]1[C:2]([S:1][CH2:20][C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][N:14]=2)=[N:3][C:4]2[C:9]([N:10]=1)=[CH:8][CH:7]=[CH:6][CH:5]=2

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 23392Picolyl chloride hydrochlorideHCID 1784186273-Methylquinoxaline-2-thiol

생성물 1

HCID 14052175HCID 14052175, 화합물수율 68.7%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

In a mixture of 70 ml of acetone and 7 ml of water were suspended 1.9 g of 2-mercapto-3-methylquinoxaline and 1.95 g of 2-picolyl chloride hydrochloride. To the suspension was added 4.0 g of potassium carbonate. The resulting mixture was stirred at room temperature for 1 hr., and the solvent was removed under reduced pressure. The residue was extracted with chloroform after addition of chloroform and water. The organic layer was separated and dried over sodium sulfate. The sodium sulfate was removed by filtration, and the filtrate was placed under reduced pressure to remove the solvent. The residue was dissolved in 20 ml of ethanol. To the solution under chilling with ice were successively added 3.2 ml of 5.2N ethanolic hydrochloric acid and ether to precipitate crystals. The crystals were collected by filtration to give 2.25 g of 3-methyl-2-(2-pyridylmethylthio)quinoxaline hydrochloride as a violet crystalline powder.

후처리

  1. custom, and the solvent was removed under reduced pressure
  2. extractionThe residue was extracted with chloroform
  3. additionafter addition of chloroform and water
  4. customThe organic layer was separated
  5. dry with materialdried over sodium sulfate
  6. customThe sodium sulfate was removed by filtration
  7. customto remove the solvent
  8. dissolutionThe residue was dissolved in 20 ml of ethanol
  9. temperatureTo the solution under chilling with ice
  10. customto precipitate crystals
  11. filtrationThe crystals were collected by filtration

출처 및 근거

ORD 기록
ord-c0f1a49cb3e24ece89478fc6e16f4f08
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05106976

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