Hydrochloric Acid → HCID 178482540, 화합물

HRID 493695

반응식

HRID 493695 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([CH2:15][CH2:16][C:17]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)=[O:18])(=[O:14])=[O:13])[CH:6]=[CH:5]2.Cl.[Cl:26][CH2:27][C:28]1[N:29]([CH3:35])/[C:30](=[N:33]/[CH3:34])/[S:31][CH:32]=1.C(=O)([O-])[O-].[K+].[K+].Cl>CN(C=O)C.C(OCC)(=O)C.CCOCC>[ClH:1].[ClH:26].[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([CH2:15][CH2:16][C:17]([N:19]1[CH2:20][CH2:21][N:22]([CH2:27][C:28]3[N:29]([CH3:35])/[C:30](=[N:33]/[CH3:34])/[S:31][CH:32]=3)[CH2:23][CH2:24]1)=[O:18])(=[O:14])=[O:13])[CH:6]=[CH:5]2

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 231308831-(3-((6-Chloro-2-naphthyl)sulfonyl)propionyl)piperazineHCID 178482537HCID 178482537, 화합물

생성물 1

HCID 178482540HCID 178482540, 화합물수율 121.4%

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

A suspension of 1-(3-((6-chloro-2-naphthyl)sulfonyl)propionyl)piperazine (2.5 g) obtained in Example 3a), N-((2Z)-4-chloromethyl-3-methyl-1,3-thiazol-2(3H)-ylidene)-N-methylamine hydrochloride (2.2 g) and potassium carbonate (2.4 g) in DMF (50 mL) was mixed at 65° C. for 3 hours. The solvent was distilled off under reduced pressure, the residue was diluted with an aqueous potassium carbonate solution, and extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The product, which was obtained by the purification of the residue with a basic silica gel column, was dissolved in ethyl acetate. A solution of hydrogen chloride in ether was added thereto, and the mixture was concentrated and dried to give the title compound (2.4 g) as a colorless powder.

후처리

  1. additionwas mixed at 65° C. for 3 hours
  2. distillationThe solvent was distilled off under reduced pressure
  3. additionthe residue was diluted with an aqueous potassium carbonate solution
  4. extractionextracted with chloroform
  5. dry with materialThe extract was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe product, which was obtained by the purification of the residue with a basic silica gel column
  8. concentrationthe mixture was concentrated
  9. customdried

출처 및 근거

ORD 기록
ord-3a3fbf0254c84df7ae80a04ae775c56e
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534887B2

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