p-Toluenesulfonyl isocyanate → 1-(4-methyl-benzenesulfonyl)-3-[3-(3-pyridin-4-yl-6,7-dihydro-5H-pyrazolo-[5,1-b][1,3]thiazin-2-yl)-phenyl]-urea

HRID 38080

반응식

HRID 38080 반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[C:8]([C:16]3[CH:17]=[C:18]([NH2:22])[CH:19]=[CH:20][CH:21]=3)=[N:9][N:10]3[CH2:15][CH2:14][CH2:13][S:12][C:11]=23)=[CH:3][CH:2]=1.[CH3:23][C:24]1[CH:29]=[CH:28][C:27]([S:30]([N:33]=[C:34]=[O:35])(=[O:32])=[O:31])=[CH:26][CH:25]=1>ClCCl>[CH3:23][C:24]1[CH:29]=[CH:28][C:27]([S:30]([NH:33][C:34]([NH:22][C:18]2[CH:19]=[CH:20][CH:21]=[C:16]([C:8]3[C:7]([C:4]4[CH:5]=[CH:6][N:1]=[CH:2][CH:3]=4)=[C:11]4[S:12][CH2:13][CH2:14][CH2:15][N:10]4[N:9]=3)[CH:17]=2)=[O:35])(=[O:32])=[O:31])=[CH:26][CH:25]=1

참가 물질

4

반응물 2

HCID 77703p-Toluenesulfonyl isocyanateHCID 674228643-(3-Pyridin-4-yl-6,7-dihydro-5H-pyrazolo[5,1-b][1,3]thiazin-2-yl)-phenylamine

생성물 1

HCID 584771051-(4-methyl-benzenesulfonyl)-3-[3-(3-pyridin-4-yl-6,7-dihydro-5H-pyrazolo-[5,1-b][1,3]thiazin-2-yl)-phenyl]-urea

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-(3-pyridin-4-yl-6,7-dihydro-5H-pyrazolo[5,1-b][1,3]thiazin-2-yl)-phenylamine (prepared as described in Example 3) (50 mg, 0.162 mmol) in dichloromethane (5 mL), 4-methyl-benzenesulfonyl isocyanate (28 mg, 0.178 mmol) was added in one portion. The reaction mixture was stirred at room temperature for 2 hours and evaporated to dryness. The reaction mixture was purified by flash chromatography over silica gel using dichloromethane-methanol (97:3) as the eluant system. 1-(4-methyl-benzenesulfonyl)-3-[3-(3-pyridin-4-yl-6,7-dihydro-5H-pyrazolo-[5,1-b][1,3]thiazin-2-yl)-phenyl]-urea was obtained as a colorless solid (21 mg, 32%).

후처리

  1. customevaporated to dryness
  2. customThe reaction mixture was purified by flash chromatography over silica gel

출처 및 근거

ORD 기록
ord-c492f94afd604fac8010e313b1faff65
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524707B2

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