Trifluoroacetic acid → N-[2-[[(2,3-Difluorophenyl)methyl]thio]-6-methoxypyrimidin-4-yl]piperazine-1-sulfonamide, trifluoroacetate salt

HRID 1024891ノート

反応式

HRID 1024891 の反応式
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][S:10][C:11]1[N:16]=[C:15]([NH:17][S:18]([N:21]2[CH2:26][CH2:25][N:24](C(OC(C)(C)C)=O)[CH2:23][CH2:22]2)(=[O:20])=[O:19])[CH:14]=[C:13]([O:34][CH3:35])[N:12]=1.[F:36][C:37]([F:42])([F:41])[C:38]([OH:40])=[O:39]>ClCCl>[F:36][C:37]([F:42])([F:41])[C:38]([OH:40])=[O:39].[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][S:10][C:11]1[N:16]=[C:15]([NH:17][S:18]([N:21]2[CH2:22][CH2:23][NH:24][CH2:25][CH2:26]2)(=[O:20])=[O:19])[CH:14]=[C:13]([O:34][CH3:35])[N:12]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 670512451,1-Dimethylethyl 4-[2-[[(2,3-difluorophenyl)methyl]thio)-6-methoxypyrimidin-4-yl sulfamoyl]piperazine-1-carboxylate

生成物 1

HCID 67051309N-[2-[[(2,3-Difluorophenyl)methyl]thio]-6-methoxypyrimidin-4-yl]piperazine-1-sulfonamide, trifluoroacetate salt

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1,1-Dimethylethyl 4-[2-[[(2,3-difluorophenyl)methyl]thio]-6-methoxypyrimidin-4-yl sulfamoyl]piperazine-1-carboxylate (the product of step i) (0.36 g) and trifluoroacetic acid (1 mL) in dichloromethane (4 mL) were stirred at room temperature for 30 min. The solvent was evaporated under reduced pressure and the residue was azeotroped with toluene (3×). The residual pale yellow solid was triturated with EtOAc, filtered and dried at 40° C. under high vacuum to give the title compound as a cream solid. Yield: 0.24 g.

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was azeotroped with toluene (3×)
  3. customThe residual pale yellow solid was triturated with EtOAc
  4. filtrationfiltered
  5. customdried at 40° C. under high vacuum

出典と根拠

ORDレコード
ord-15e643d767d946beaf324731e3394a46
出典データセット
uspto-grants-2014_05
特許番号
US08722883B2

反応ノート

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