Methane → HCID 54674795, 화합물

HRID 2251806노트

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HRID 2251806 반응식
[ClH:1].[CH2:2]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[N:16]=[CH:15][C:14]([NH:17][S:18]([C:21]3[CH:26]=[CH:25][C:24]([CH:27]([CH3:29])[CH3:28])=[CH:23][CH:22]=3)(=[O:20])=[O:19])=[CH:13][CH:12]=2)[CH2:7][CH:6]1[CH3:30])[CH:3]=[CH2:4].C>C(OCC)(=O)C.[Pd]>[ClH:1].[CH:27]([C:24]1[CH:25]=[CH:26][C:21]([S:18]([NH:17][C:14]2[CH:15]=[N:16][C:11]([N:8]3[CH2:9][CH2:10][N:5]([CH2:2][CH2:3][CH3:4])[CH:6]([CH3:30])[CH2:7]3)=[CH:12][CH:13]=2)(=[O:20])=[O:19])=[CH:22][CH:23]=1)([CH3:29])[CH3:28]

참가 물질

5

반응물 2

HCID 297MethaneHCID 54674793HCID 54674793, 화합물

생성물 1

HCID 54674795HCID 54674795, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

100 mg (0.24 mmol) of N-[6-(4-allyl-3-methylpiperazin-1-yl)pyridin-3-yl]-4-isopropylbenzenesulfonamide hydrochloride from Example 13.4 were dissolved in 10 ml of ethyl acetate, after which 10 mg of palladium on active charcoal (10%) were added and the mixture was stirred overnight at room temperature under a hydrogen atmosphere. After that, the catalyst was filtered off and the filtrate was evaporated down to dryness. After 1 ml of dichloromethane had been added to the resulting residue, diethyl ether was slowly added dropwise until the solution became cloudy. The reaction mixture was stirred for 30 minutes and the precipitate which had formed was filtered off with suction. The filtrate was evaporated down to dryness, after which the residue was dissolved in a 1:1 mixture of dichloromethane and diethyl ether and converted into the hydrochloride by adding ethereal hydrochloric acid. 71 mg (63% of theory) of the title compound were obtained.

후처리

  1. filtrationAfter that, the catalyst was filtered off
  2. customthe filtrate was evaporated down to dryness
  3. additionAfter 1 ml of dichloromethane had been added to the resulting residue, diethyl ether
  4. additionwas slowly added dropwise until the solution
  5. stirringThe reaction mixture was stirred for 30 minutes
  6. customthe precipitate which had formed
  7. filtrationwas filtered off with suction
  8. customThe filtrate was evaporated down to dryness
  9. dissolutionafter which the residue was dissolved in a 1:1 mixture of dichloromethane and diethyl ether
  10. additionby adding ethereal hydrochloric acid

출처 및 근거

ORD 기록
ord-35a00cdb458145a09a87e2a8e8fbbb93
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07320979B2

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