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Potassium Carbonate → HCID 19973443, 화합물

HRID 1440245
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HRID 1440245 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][S:6][CH2:7][C:8]1[CH:9]=[CH:10][C:11]2[N:12]([CH:14]=[C:15]([CH3:17])[N:16]=2)[CH:13]=1.ClC1C=CC=C(C(OO)=[O:26])C=1.S([O-])([O-])(=O)=S.[Na+].[Na+].C(=O)([O-])[O-].[K+].[K+]>ClCCl.ClC1C=CC=C(C(OO)=O)C=1>[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][S:6]([CH2:7][C:8]1[CH:9]=[CH:10][C:11]2[N:12]([CH:14]=[C:15]([CH3:17])[N:16]=2)[CH:13]=1)=[O:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 24477Sodium ThiosulfateHCID 70297m-Chloroperbenzoic acidHCID 19973464HCID 19973464, 화합물

생성물 1

HCID 19973443HCID 19973443, 화합물수율 79.7%

시약·촉매·용매 2

HCID 70297m-Chloroperbenzoic acid
촉매
HCID 6344Dichloromethane용매2회

실험 절차

4.95 g of the 6-((4-chlorobutyl)thiomethyl)-2-methylimidazo[1,2-a]pyridine prepared in the Preparative Example 17 was dissolved in 50 ml of dichloromethane, followed by the cooling of the obtained solution with ice. A solution of 3.18 g of m-chloroperbenzoic acid in 20 ml of dichloromethane was dropped into the resulting solution in 20 minutes. After one hour, 0.16 g of m-chloroperbenzoic acid was further added to the obtained mixture. The obtained mixture was additionally stirred for 30 minutes, followed by the addition of an aqueous solution of sodium thiosulfate. The obtained mixture was vigorously stirred at room temperature for 15 minutes, followed by the addition of an aqueous solution of potassium carbonate. The obtained mixture was extracted with dichloromethane. The organic phase was dried over anhydrous potassium carbonate and distilled to remove the solvent. The residue was purified by silica gel column chromatography [solvent: dichloromethane/methanol (50:1 to 80:1)] to give 4.18 g of the title compound as a pale-pink solid (yield: 79%).

후처리

  1. temperaturecooling of the obtained solution with ice
  2. stirringThe obtained mixture was vigorously stirred at room temperature for 15 minutes
  3. extractionThe obtained mixture was extracted with dichloromethane
  4. dry with materialThe organic phase was dried over anhydrous potassium carbonate
  5. distillationdistilled
  6. customto remove the solvent
  7. customThe residue was purified by silica gel column chromatography [solvent: dichloromethane/methanol (50:1 to 80:1)]

출처 및 근거

ORD 기록
ord-63554cd10d9a460aa464ec1eeed2ecea
출처 데이터셋
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05498634

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