Butyl iodide → Methyl Z-4-[[2-butyl-5-[(1-butyl-2,5-dioxo-4-imidazolidinylidene)methyl]-1H-imidazol-1-yl]methyl]benzoate

HRID 1033111

반응식

HRID 1033111 반응식
[O:1]=[C:2]1[N:6]=[C:5](P(=O)(OCC)OCC)[C:4](=[O:15])[NH:3]1.C([O-])([O-])=O.[K+].[K+].I[CH2:23][CH2:24][CH2:25][CH3:26].[CH2:27]([C:31]1[N:32]([CH2:38][C:39]2[CH:48]=[CH:47][C:42]([C:43]([O:45][CH3:46])=[O:44])=[CH:41][CH:40]=2)[C:33]([CH:36]=O)=[CH:34][N:35]=1)[CH2:28][CH2:29][CH3:30]>CN(C=O)C.O.C(Cl)Cl>[CH2:27]([C:31]1[N:32]([CH2:38][C:39]2[CH:48]=[CH:47][C:42]([C:43]([O:45][CH3:46])=[O:44])=[CH:41][CH:40]=2)[C:33](/[CH:36]=[C:5]2\[NH:6][C:2](=[O:1])[N:3]([CH2:23][CH2:24][CH2:25][CH3:26])[C:4]\2=[O:15])=[CH:34][N:35]=1)[CH2:28][CH2:29][CH3:30]

참가 물질

8

반응물 4

HCID 10962Butyl iodideHCID 11430Potassium CarbonateHCID 10334966Methyl 4-[(2-butyl-5-formyl-1H-imidazol-1-YL)methyl]benzoateHCID 53733419Diethyl (2,5-dioxo-2,5-dihydro-1H-imidazol-4-yl)phosphonate

생성물 1

HCID 11743857Methyl Z-4-[[2-butyl-5-[(1-butyl-2,5-dioxo-4-imidazolidinylidene)methyl]-1H-imidazol-1-yl]methyl]benzoate

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

To a solution of diethyl 2,5-dioxo-4-imidazolylphosphonate (1.5 g, 0.33 mmol) in DMF (4 mL) is added K2CO3 and then 1-iodobutane (0.79 mL, 6.96 mmol). This mixture is stirred for 16 hours at room temperature. To this yellow mixture is added methyl 4-[(2-butyl-5-formyl-1H-imidazol-1-yl)methyl]benzoate (1.05 g, 3.5 mmol). After 2 hours methylene chloride (10 mL) was added to aid stirring. The mixture was stirred for 16 hours. After diluting the reaction mixture with water it was extracted with ethyl acetate. This extract was washed with water and brine. The extract was dried over MgSO4, filtered and then concentrated until crystallization was apparent. The solid was collected and dried.

후처리

  1. stirringstirring
  2. stirringThe mixture was stirred for 16 hours
  3. extractionwas extracted with ethyl acetate
  4. washThis extract was washed with water and brine
  5. dry with materialThe extract was dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated until crystallization
  8. customThe solid was collected
  9. customdried

출처 및 근거

ORD 기록
ord-d6ec9288e119447dbbac5aa643d34671
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05308853

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