1,1'-Carbonyldiimidazole → HCID 22717700、化合物

HRID 1582553

反応式

HRID 1582553 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][C:10]([NH:12][OH:13])=[O:11].[C:14](N1C=CN=C1)(N1C=CN=C1)=[O:15]>O1CCCC1>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[N:9]1[C:14](=[O:15])[O:13][NH:12][C:10]1=[O:11]

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 42954891-(2,4-Dichlorophenyl)-3-hydroxyurea

生成物 1

HCID 22717700HCID 22717700、化合物収率 81%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
25 °C

実験手順

A solution of 4.2 g (19 mmol) of the compound of step A in tetrahydrofuran (20 mL) was treated with carbonyldiimidazole (3.2 g, 19 mmol). The mixture was stirred at 25° C. for 16 h. Some precipitated imidazole was filtered off and the filtrate was concentrated under reduced pressure. The residue was partitioned between 1N HCl (20 mL) and ethyl acetate (50 mL). The organic layer was dried over magnesium sulfate and concentrated to an oil which solidified to give 3.8 g of the title compound of Step B as a solid melting at 104-107° C. It was used directly for the next step without further purification.

後処理

  1. filtrationSome precipitated imidazole was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was partitioned between 1N HCl (20 mL) and ethyl acetate (50 mL)
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated to an oil which

出典と根拠

ORDレコード
ord-b6435057ee3243468fa500dc1212dba6
出典データセット
uspto-grants-2004_05
特許番号
US06737383B1

関連ノート

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