Sodium Dithionite → HCID 57747382、化合物

HRID 386641ノート

反応式

HRID 386641 の反応式
[O-]S(S([O-])=O)=O.[Na+].[Na+].[Br:9][C:10]1[CH:15]=[C:14]([CH3:16])[C:13]([S:17][C:18]2[C:23]([N+]([O-])=O)=[C:22](/[CH:27]=[CH:28]/[N:29](C)C)[N:21]=[C:20]([N:32]([C:40]3[CH:45]=[CH:44][C:43]([C:46]#[N:47])=[CH:42][CH:41]=3)[C:33](=[O:39])[O:34][C:35]([CH3:38])([CH3:37])[CH3:36])[N:19]=2)=[C:12]([CH3:48])[CH:11]=1>O.C1COCC1>[Br:9][C:10]1[CH:11]=[C:12]([CH3:48])[C:13]([S:17][C:18]2[C:23]3[NH:29][CH:28]=[CH:27][C:22]=3[N:21]=[C:20]([N:32]([C:40]3[CH:45]=[CH:44][C:43]([C:46]#[N:47])=[CH:42][CH:41]=3)[C:33](=[O:39])[O:34][C:35]([CH3:38])([CH3:37])[CH3:36])[N:19]=2)=[C:14]([CH3:16])[CH:15]=1

参加物

5

反応物 2

HCID 24489Sodium DithioniteHCID 57747434HCID 57747434、化合物

生成物 1

HCID 57747382HCID 57747382、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of Na2S2O4 (230 mmol) in water (100 ml) is added to a solution of tert-butyl 4-(4-bromo-2,6-dimethylphenylthio)-6-((E)-2-(dimethylamino)vinyl)-5-nitropyrimidin-2-yl4-cyanophenylcarbamate (46 mmol) in THF (300 ml). The mixture is stirred at room temperature for 2 days and then concentrated. The residue is washed with water and extracted with ethyl acetate. The organic layer is concentrated and the product obtained by crystallization from a mixture of water and methanol.

後処理

  1. concentrationconcentrated
  2. washThe residue is washed with water
  3. extractionextracted with ethyl acetate
  4. concentrationThe organic layer is concentrated
  5. customthe product obtained by crystallization from a mixture of water and methanol

出典と根拠

ORDレコード
ord-791204a91cb04c3ab8806628f9487a6e
出典データセット
uspto-grants-2013_02
特許番号
US08372852B2

反応ノート

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