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

HRID 1024891노트

반응식

HRID 1024891 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-15e643d767d946beaf324731e3394a46
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722883B2

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