Hydrochloric Acid → Methyl Z-4-[[2-butyl-5-[[1-butyl-3-[(3,5-dimethyl-4-isoxazolyl)methyl]-2,5-dioxo-4-imidazolidinylidene]methyl]-1H-imidazol-1-yl]methyl]benzoate monohydrochloride

HRID 1033118노트

반응식

HRID 1033118 반응식
[CH2:1]([C:5]1[N:6]([CH2:30][C:31]2[CH:40]=[CH:39][C:34]([C:35]([O:37][CH3:38])=[O:36])=[CH:33][CH:32]=2)[C:7](/[CH:10]=[C:11]2\[N:12]([CH2:22][C:23]3[C:24]([CH3:29])=[N:25][O:26][C:27]=3[CH3:28])[C:13](=[O:21])[N:14]([CH2:17][CH2:18][CH2:19][CH3:20])[C:15]\2=[O:16])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4].C([O-])([O-])=O.[K+].[K+].[Cl:47]CC1C(C)=NOC=1C.Cl>CN(C=O)C.CCOCC>[ClH:47].[CH2:1]([C:5]1[N:6]([CH2:30][C:31]2[CH:32]=[CH:33][C:34]([C:35]([O:37][CH3:38])=[O:36])=[CH:39][CH:40]=2)[C:7](/[CH:10]=[C:11]2\[N:12]([CH2:22][C:23]3[C:24]([CH3:29])=[N:25][O:26][C:27]=3[CH3:28])[C:13](=[O:21])[N:14]([CH2:17][CH2:18][CH2:19][CH3:20])[C:15]\2=[O:16])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 88246Isoxazole, 4-(chloromethyl)-3,5-dimethyl-HCID 11757216methyl Z-4-[[2-butyl-5-[[1-butyl-3-[(3,5-dimethyl-4-isoxazolyl)methyl]-2,5-dioxo-4-imidazolidinylidene]methyl]-1H-imidazol-1-yl]methyl]benzoate

생성물 1

HCID 19919836Methyl Z-4-[[2-butyl-5-[[1-butyl-3-[(3,5-dimethyl-4-isoxazolyl)methyl]-2,5-dioxo-4-imidazolidinylidene]methyl]-1H-imidazol-1-yl]methyl]benzoate monohydrochloride

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of methyl Z-4-[[2-butyl-5-[[1-butyl-3-[(3,5-dimethyl-4-isoxazolyl)methyl]-2,5-dioxo-4-imidazolidinylidene]methyl]-1H-imidazol-1-yl]methyl]benzoate (1.00 g, 2.281 mmol) in DMF (10 mL) is added K2CO3 (1.580 g, 0.011 moles). After stirring for 15 minutes 4-chloromethyl-3,5-dimethylisoxazole (0.35 g, 2.39 mmol) is added. The mixture is stirred for 24 hours. The solvents were removed under high vacuum. After diluting with ethyl acetate and washing with water and brine the solution is dried over MgSO4. Evaporation in vacuo affords a viscous oil which is dissolved in ether and treated with ethereal HCl to afford a foamy solid upon evaporation in vacuo. This solid is crystallized from ethyl acetate/hexane.

후처리

  1. additionis added
  2. customThe solvents were removed under high vacuum
  3. additionAfter diluting with ethyl acetate
  4. washwashing with water and brine the solution
  5. dry with materialis dried over MgSO4
  6. customEvaporation in vacuo
  7. customaffords a viscous oil which
  8. customto afford a foamy solid
  9. customupon evaporation in vacuo
  10. customThis solid is crystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-c9554336a2ce4a7a911e64670e87e6e2
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05308853

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