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Hydrochloric Acid → Methyl 2-butyl-1-[(2'-carboxybiphenyl-4-yl)methyl]-4-(methoxymethyl)imidazole-5-carboxylate

HRID 52883
ノート
印刷プレビュー

反応式

HRID 52883 の反応式
C([O:5][C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[CH:19]=[CH:18][C:17]([CH2:20][N:21]2[C:25]([C:26]([O:28][CH3:29])=[O:27])=[C:24]([CH2:30][O:31][CH3:32])[N:23]=[C:22]2[CH2:33][CH2:34][CH2:35][CH3:36])=[CH:16][CH:15]=1)=[O:7])(C)(C)C.Cl>O1CCOCC1>[CH2:33]([C:22]1[N:21]([CH2:20][C:17]2[CH:16]=[CH:15][C:14]([C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=3[C:6]([OH:7])=[O:5])=[CH:19][CH:18]=2)[C:25]([C:26]([O:28][CH3:29])=[O:27])=[C:24]([CH2:30][O:31][CH3:32])[N:23]=1)[CH2:34][CH2:35][CH3:36]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 19036253Methyl 1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-2-butyl-4-(methoxymethyl)imidazole-5-carboxylate

生成物 1

HCID 19036151Methyl 2-butyl-1-[(2'-carboxybiphenyl-4-yl)methyl]-4-(methoxymethyl)imidazole-5-carboxylate収率 97.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution of 0.30 g of methyl 1-[(2'-t-butoxycarbonylbiphenyl-4-yl)methyl]-2-butyl-4-(methoxymethyl)imidazole-5-carboxylate (prepared as described in Example 8) in 3 ml of a 4N solution of hydrogen chloride in dioxane was allowed no stand at room temperature for 5 hours, after which the solvent was removed by distillation under reduced pressure. The syrupy residue was triturated in diethyl ether and collected by filtration, to give 0.26 g of the title compound in the form of its hydrochloride, melting at 106°-110° C. (with softening).

後処理

  1. customat room temperature
  2. customfor 5 hours
  3. customafter which the solvent was removed by distillation under reduced pressure
  4. customThe syrupy residue was triturated in diethyl ether
  5. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-3c3265b24db644e8a6eb50a4a367af8a
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05616599

反応ノート

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