Trifluoroacetic acid → N-[2-[[(2,3-difluorophenyl)methyl]thio]-6-ethoxy-4-pyrimidinyl]-1-piperazinesulfonamide

HRID 1175364노트

반응식

HRID 1175364 반응식
CC(OC([N:8]1[CH2:13][CH2:12][N:11]([S:14]([NH:17][C:18]2[CH:23]=[C:22]([O:24][CH2:25][CH3:26])[N:21]=[C:20]([S:27][CH2:28][C:29]3[CH:34]=[CH:33][CH:32]=[C:31]([F:35])[C:30]=3[F:36])[N:19]=2)(=[O:16])=[O:15])[CH2:10][CH2:9]1)=O)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[F:36][C:30]1[C:31]([F:35])=[CH:32][CH:33]=[CH:34][C:29]=1[CH2:28][S:27][C:20]1[N:19]=[C:18]([NH:17][S:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)(=[O:16])=[O:15])[CH:23]=[C:22]([O:24][CH2:25][CH3:26])[N:21]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 536283464-[[[2-[[(2,3-Difluorophenyl)methyl]thio]-6-ethoxy-4-pyrimidinyl]amino]sulfonyl]-1-piperazinecarboxylic acid-1,1-dimethylethyl ester

생성물 1

HCID 59558798N-[2-[[(2,3-difluorophenyl)methyl]thio]-6-ethoxy-4-pyrimidinyl]-1-piperazinesulfonamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-[[[2-[[(2,3-difluorophenyl)methyl]thio]-6-ethoxy-4-pyrimidinyl]amino]sulfonyl]-1-piperazinecarboxylic acid-1,1-dimethylethyl ester (the product from step ii) (0.24 g) in DCM (2 mL) was added trifluoroacetic acid (2 mL) and the reaction mixture was stirred at ambient temperature for 2.5 h. The reaction mixture was evaporated, the residue was azeotroped with DCM (×2) and then purified by reverse phase HPLC eluting with acetonitrile/aq. 0.2% trifluoroacetic acid mixtures to give title compound as a white solid. Yield: 0.18 g

후처리

  1. customThe reaction mixture was evaporated
  2. customthe residue was azeotroped with DCM (×2)
  3. custompurified by reverse phase HPLC
  4. washeluting with acetonitrile/aq

출처 및 근거

ORD 기록
ord-7fdacd03e14f426b81e477bbec0dd66e
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07838675B2

반응 노트

불러오는 중…