Sodium Dithionite → HCID 57747382、化合物

HRID 222085ノート

反応式

HRID 222085 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-abf0299216134cd090b31288af5e4858
出典データセット
uspto-grants-2012_06
特許番号
US08207178B2

反応ノート

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