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

HRID 1175450ノート

反応式

HRID 1175450 の反応式
[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

参加物

4

反応物 2

HCID 431320453-Oxopiperazine-1-sulfonamideHCID 866198774-Chloro-2-([(2,3-difluorophenyl)methyl]thio]-6-methoxypyrimidine2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4a45153d6d3e44f1a0bc9643ff32343f
出典データセット
uspto-grants-2010_11
特許番号
US07838675B2

反応ノート

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