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2-n-Propyl-5-(2-aminoethyl)-3-[2'(1-trityl-1H-tetrazol-5-yl)biphenyl-4-yl]methylimidazole → HCID 178439974、化合物

HRID 1655119
ノート
印刷プレビュー

反応式

HRID 1655119 の反応式
[CH2:1]([C:4]1[N:5]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25]3[N:29](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:28]=[N:27][N:26]=3)=[CH:15][CH:14]=2)[CH:6]=[C:7]([CH2:9][CH2:10][NH2:11])[N:8]=1)[CH2:2][CH3:3].O.[C:50]([O:54][CH2:55][CH3:56])(=[O:53])[CH:51]=[O:52].C([OH:59])C.Cl>O1CCCC1>[C:50]([OH:54])(=[O:53])[C:51]([OH:59])=[O:52].[CH2:1]([C:4]1[N:5]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25]3[NH:29][N:28]=[N:27][N:26]=3)=[CH:15][CH:14]=2)[C:6]2[CH:51]([C:50]([O:54][CH2:55][CH3:56])=[O:53])[NH:11][CH2:10][CH2:9][C:7]=2[N:8]=1)[CH2:2][CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 199329822-n-Propyl-5-(2-aminoethyl)-3-[2'(1-trityl-1H-tetrazol-5-yl)biphenyl-4-yl]methylimidazoleHCID 21887872Ethanol hydrochlorideHCID 22414697Ethyl glyoxylate hydrate

生成物 1

HCID 178439974HCID 178439974、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a mixture of 2-n-propyl-4-(2-aminoethyl)-1-[2'-(1-trityl-1H-tetrazol-5-yl)biphenyl-4-yl)methylimidazole (21.95 g) and tetrahydrofuran (200 ml) is added a solution of ethyl glyoxylate hydrate (4.25 g) in tetrahydrofuran (20 ml) at 5° C. The mixture is stirred overnight at room temperature and refluxed for 30 minutes. To a mixture is added a 8% hydrogen chloride ethanol solution (100 ml) at room temperature. The reaction mixture is stirred for 30 minutes, then evaporated. The residue is dissolved in chloroform and washed successively with a saturated sodium hydrogen carbonate solution and brine. The organic layer is dried and evaporated. The oxalate is recrystallized from ethanol to give ethyl 2-n-propyl-3-[2'-(1H-tetrazol-5-yl)biphenyl-4-yl]methyl-4,5,6,7-tetrahydroimidazo[4,5-c]pyridine-4-carboxylate oxalate (10.84 g).

後処理

  1. temperaturerefluxed for 30 minutes
  2. stirringThe reaction mixture is stirred for 30 minutes
  3. customevaporated
  4. dissolutionThe residue is dissolved in chloroform
  5. washwashed successively with a saturated sodium hydrogen carbonate solution and brine
  6. customThe organic layer is dried
  7. customevaporated
  8. customThe oxalate is recrystallized from ethanol

出典と根拠

ORDレコード
ord-c9bc6ae52d6348d389c44eb2dddd1309
出典データセット
uspto-grants-1995_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05409936

反応ノート

読み込み中…

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