Trifluoroacetic acid → HCID 19972885, 화합물

HRID 2260650노트

반응식

HRID 2260650 반응식
[C:1]1([S:11]([NH:14][CH2:15][CH2:16][O:17][CH:18]2[CH2:23][CH2:22][CH2:21][CH2:20][C:19]2([C:37]2[CH:38]=[CH:39][C:40]3[N:41]([CH:43]=[CH:44][N:45]=3)[CH:42]=2)[C:24]([S:27]CC2C=CC(OC)=CC=2)=[N:25][CH3:26])(=[O:13])=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.C1(OC)C=CC=CC=1.FC(F)(F)C(O)=O.C(=O)([O-])[O-].[Na+].[Na+]>ClCCl>[C:1]1([S:11]([NH:14][CH2:15][CH2:16][O:17][CH:18]2[CH2:23][CH2:22][CH2:21][CH2:20][C:19]2([C:37]2[CH:38]=[CH:39][C:40]3[N:41]([CH:43]=[CH:44][N:45]=3)[CH:42]=2)[C:24](=[S:27])[NH:25][CH3:26])(=[O:12])=[O:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 10340Sodium CarbonateHCID 19972903HCID 19972903, 화합물

생성물 1

HCID 19972885HCID 19972885, 화합물수율 65%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture comprising 0.4 g of the 2-(2-(1-naphthalenesulfonamido)ethoxy)-1-(imidazo[1,2-a]-pyridin-6-yl)-1-((4-methoxybenzylthio)(methylimino)methyl)cyclohexane, 0.5 ml of anisole, 5 ml of trifluoroacetic acid and 5 ml of dichloromethane was stirred under cooling with ice for 1.5 hours, followed by the addition of ice-water. The resulting mixture was alkalinized with sodium carbonate and extracted with chloroform. The chloroform phase was dried over anhydrous magnesium sulfate and ditilled to remove the solvent. The residue was purified by silica gel column chromatography (solvent:a 30:1 dichloromethane/methanol mixture) and crystallized from ethyl acetate/n-hexane to give 0.21 g of the title compound as a white powder (yield: 65%).

후처리

  1. temperatureunder cooling with ice for 1.5 hours
  2. extractionextracted with chloroform
  3. dry with materialThe chloroform phase was dried over anhydrous magnesium sulfate
  4. customto remove the solvent
  5. customThe residue was purified by silica gel column chromatography (solvent
  6. customa 30:1 dichloromethane/methanol mixture) and crystallized from ethyl acetate/n-hexane

출처 및 근거

ORD 기록
ord-c61ece50250c41bfbebaf646d5d4c3f3
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05478839

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