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

HRID 1958913ノート

反応式

HRID 1958913 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-95dc3351a83c4461a30e91f4ba708902
出典データセット
uspto-grants-2013_04
特許番号
US08410123B2

反応ノート

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