3-Oxopiperazine-1-sulfonamide → N-[2-[[(2,3-Difluorophenyl)methyl]thio]-6-methoxypyrimidin-4-yl]-3-oxopiperazine-1-sulfonamide

HRID 1175450노트

반응식

HRID 1175450 반응식
[O:1]=[C:2]1[NH:7][CH2:6][CH2:5][N:4]([S:8]([NH2:11])(=[O:10])=[O:9])[CH2:3]1.Cl[C:13]1[CH:18]=[C:17]([O:19][CH3:20])[N:16]=[C:15]([S:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([F:29])[C:24]=2[F:30])[N:14]=1>CCOC(C)=O>[F:30][C:24]1[C:25]([F:29])=[CH:26][CH:27]=[CH:28][C:23]=1[CH2:22][S:21][C:15]1[N:14]=[C:13]([NH:11][S:8]([N:4]2[CH2:5][CH2:6][NH:7][C:2](=[O:1])[CH2:3]2)(=[O:10])=[O:9])[CH:18]=[C:17]([O:19][CH3:20])[N:16]=1

참가 물질

4

반응물 2

HCID 431320453-Oxopiperazine-1-sulfonamideHCID 866198774-Chloro-2-([(2,3-difluorophenyl)methyl]thio]-6-methoxypyrimidine2회

생성물 1

HCID 59558765N-[2-[[(2,3-Difluorophenyl)methyl]thio]-6-methoxypyrimidin-4-yl]-3-oxopiperazine-1-sulfonamide

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

The title compound was prepared from 3-oxopiperazine-1-sulfonamide (the product of step i) (0.22 g) and 4-chloro-2-[[(2,3-difluorophenyl)methyl]thio]-6-methoxypyrimidine (the product of Example 35, step i) (0.25 g) according to the procedure outlined in Example 1, step iv). The crude material was purified by column chromatography using EtOAc/isohexane (1:1) as eluent to give a white solid. This solid was dissolved in EtOAc and Et2O and extracted with 1N sodium hydroxide. The basic solution was washed with Et2O, acidified with dilute hydrochloric acid and extracted with EtOAc. The organic solution was washed with H2O, dried (MgSO4) and the solvent evaporated in vacuo to give the product as a yellow foam.

후처리

  1. customThe crude material was purified by column chromatography
  2. customto give a white solid
  3. extractionEt2O and extracted with 1N sodium hydroxide
  4. washThe basic solution was washed with Et2O
  5. extractionextracted with EtOAc
  6. washThe organic solution was washed with H2O
  7. dry with materialdried (MgSO4)
  8. customthe solvent evaporated in vacuo

출처 및 근거

ORD 기록
ord-4a45153d6d3e44f1a0bc9643ff32343f
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07838675B2

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