Sulfuric Acid → HCID 71252301、化合物

HRID 2412053ノート

反応式

HRID 2412053 の反応式
[O:1]=[C:2]1[NH:6][CH2:5][CH2:4][N:3]1[C:7]1[CH:8]=[CH:9][C:10]([C:15]([N:17]2[CH2:22][CH2:21][N:20]([C:23]3[C:28]([CH3:29])=[CH:27][C:26]([CH3:30])=[C:25]([CH3:31])[N:24]=3)[CH2:19][CH2:18]2)=[O:16])=[C:11]([CH:14]=1)[C:12]#[N:13].FC(F)(F)C(O)=[O:35].S(=O)(=O)(O)O.[OH-].[Na+]>O>[O:1]=[C:2]1[NH:6][CH2:5][CH2:4][N:3]1[C:7]1[CH:8]=[CH:9][C:10]([C:15]([N:17]2[CH2:18][CH2:19][N:20]([C:23]3[C:28]([CH3:29])=[CH:27][C:26]([CH3:30])=[C:25]([CH3:31])[N:24]=3)[CH2:21][CH2:22]2)=[O:16])=[C:11]([CH:14]=1)[C:12]([NH2:13])=[O:35]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 71252151HCID 71252151、化合物

生成物 1

HCID 71252301HCID 71252301、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
10 °C

実験手順

5-(2-Oxoimidazolidin-1-yl)-2-[4-(3,5,6-trimethylpyridin-2-yl)piperazine-1-carbonyl]benzonitrile (418 mg) described in Example 445 was added to a solution of trifluoroacetic acid (1.12 mL) and concentrated sulfuric acid (0.28 mL) under cooling, and the mixture was stirred at 10° C. for 1 hr. Then, the reaction mixture was added to water under ice-cooling, neutralized with 4N aqueous sodium hydroxide solution and the to mixture was stirred for 1 hr. The obtained precipitate was collected by filtration to give the title compound (363 mg).

後処理

  1. temperatureunder cooling
  2. stirringthe to mixture was stirred for 1 hr
  3. filtrationThe obtained precipitate was collected by filtration

出典と根拠

ORDレコード
ord-88c29b9ed6474b9f8471dd4d459913a0
出典データセット
uspto-grants-2014_08
特許番号
US08816079B2

反応ノート

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