1,1'-Carbonyldiimidazole → HCID 22717700, 화합물

HRID 1582553

반응식

HRID 1582553 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 22717700HCID 22717700, 화합물수율 81%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b6435057ee3243468fa500dc1212dba6
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06737383B1

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