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

HRID 1648516
ノート
印刷プレビュー

反応式

HRID 1648516 の反応式
[CH2:1]([C:5]1[N:6]([CH2:22][C:23]2[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[CH:25][CH:24]=2)[C:7](/[CH:10]=[C:11]2\[NH:12][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+].[ClH:39].[NH2:40][C:41]1[S:42][CH:43]=[C:44]([CH2:46][Cl:47])[N:45]=1.Cl>CN(C=O)C.CCOCC>[ClH:47].[ClH:39].[CH2:1]([C:5]1[N:6]([CH2:22][C:23]2[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[CH:25][CH:24]=2)[C:7](/[CH:10]=[C:11]2\[N:12]([CH2:46][C:44]3[N:45]=[C:41]([NH2:40])[S:42][CH:43]=3)[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 732282-Thiazolamine, 4-(chloromethyl)-, hydrochloride (1:1)HCID 11743857Methyl Z-4-[[2-butyl-5-[(1-butyl-2,5-dioxo-4-imidazolidinylidene)methyl]-1H-imidazol-1-yl]methyl]benzoate

生成物 1

HCID 19919807Methyl Z-4-[[2-butyl-5-[[1-butyl-3-[(2-amino-4-thiazolyl)methyl]-2,5-dioxo-4-imidazolidinylidene]methyl]-1H-imidazol-1-yl]methyl]benzoate dihydrochloride

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-2,5-dioxo-4-imidazolidinylidene)methyl]-1H-imidazol-1-yl]methyl]benzoate (0.569 g, 1.2 mmol) in DMF (5 mL) is added K2CO3 (2.0 g, 15 mmol). After stirring for 5 minutes 2-amino-4-chloromethylthiazole hydrochloride (0.222 g, 1.2 mmol) is added. The mixture is stirred for 48 hours and then filtered. The filtrate is concentrated in vacuo and dissolved in methylene chloride (30 mL). This solution is washed with water and dried over K2CO3 and charcoal. A viscous oil is obtained by evaporation of the solvents in vacuo. This oil is dissolved in ether and treated with ethereal HCl to precipitate a gum which is collected by decantation. This gum is recrystallized from 2-propanol/ether.

後処理

  1. additionis added
  2. filtrationfiltered
  3. concentrationThe filtrate is concentrated in vacuo
  4. dissolutiondissolved in methylene chloride (30 mL)
  5. washThis solution is washed with water
  6. dry with materialdried over K2CO3 and charcoal
  7. customA viscous oil is obtained by evaporation of the solvents in vacuo
  8. customto precipitate a gum which
  9. customis collected by decantation
  10. customThis gum is recrystallized from 2-propanol/ether

出典と根拠

ORDレコード
ord-83b7ef2b04c342428c346c9f5a5563ff
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05436260

反応ノート

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