Diisopropylethylamine → HCID 71252181, 화합물

HRID 2411226

반응식

HRID 2411226 반응식
[NH2:1][C:2]1[C:3]([CH3:9])=[CH:4][C:5]([CH3:8])=[N:6][CH:7]=1.C(N(CC)C(C)C)(C)C.Cl[CH2:20][CH2:21][N:22]([CH2:33][CH2:34]Cl)[S:23]([C:26]1[CH:31]=[CH:30][C:29]([CH3:32])=[CH:28][CH:27]=1)(=[O:25])=[O:24]>O>[CH3:9][C:3]1[CH:4]=[C:5]([CH3:8])[N:6]=[CH:7][C:2]=1[N:1]1[CH2:34][CH2:33][N:22]([S:23]([C:26]2[CH:27]=[CH:28][C:29]([CH3:32])=[CH:30][CH:31]=2)(=[O:25])=[O:24])[CH2:21][CH2:20]1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 96039N,N-bis(2-chloroethyl)-p-toluenesulphonamideHCID 70606694,6-Dimethylpyridin-3-amine

생성물 1

HCID 71252181HCID 71252181, 화합물수율 15.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 5-amino-2,4-dimethylpyridine (883 mg) were added N,N-diisopropylethylamine (2.1 mL) and N,N-bis(2-chloroethyl)-p-toluenesulfonamide (2.08 g), and the mixture was stirred with heating under reflux. After completion of the reaction, water was added to the reaction mixture, the mixture was extracted with chloroform, and the solvent was evaporated. The obtained residue was purified by column chromatography (chloroform:methanol) to give 1-(4,6-dimethylpyridin-3-yl)-4-(toluene-4-sulfonyl)piperazine (380 mg). The obtained 1-(4,6-dimethylpyridin-3-yl)-4-(toluene-4-sulfonyl)piperazine (380 mg) was dissolved in acetic acid (2 mL), 40% hydrobromic acid (2 mL) was added, and the mixture was stirred at 100° C. After completion of the reaction, the reaction mixture was neutralized with aqueous sodium hydroxide solution, and the mixture was extracted with ethyl acetate. The solvent was evaporated from the organic layer to give the title compound (131 mg).

후처리

  1. temperaturewith heating
  2. temperatureunder reflux
  3. additionwas added to the reaction mixture
  4. extractionthe mixture was extracted with chloroform
  5. customthe solvent was evaporated
  6. customThe obtained residue was purified by column chromatography (chloroform:methanol)

출처 및 근거

ORD 기록
ord-eb0674f3edd244f3995b85e2b604a5a1
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08816079B2

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