Hydrochloric Acid → HCID 178482540、化合物

HRID 493695

反応式

HRID 493695 の反応式
[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

参加物

8

反応物 4

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

生成物 1

HCID 178482540HCID 178482540、化合物収率 121.4%

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3a3fbf0254c84df7ae80a04ae775c56e
出典データセット
uspto-grants-2009_05
特許番号
US07534887B2

関連ノート

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