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 1033118ノート

反応式

HRID 1033118 の反応式
[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]

参加物

7

反応物 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

生成物 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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c9554336a2ce4a7a911e64670e87e6e2
出典データセット
uspto-grants-1994_05
特許番号
US05308853

反応ノート

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