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Ethyl Acetate → 2-(1-(2-amino-2-phenylacetyl)-4-piperidinyl)-5-methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one

HRID 1162304
ノート
印刷プレビュー

反応式

HRID 1162304 の反応式
[CH3:1][C:2]1[N:6]2[C:7](=[O:33])[N:8]([CH:10]3[CH2:15][CH2:14][N:13]([C:16](=[O:32])[CH:17]([NH:24]C(=O)OC(C)(C)C)[C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[CH2:12][CH2:11]3)[CH2:9][C:5]2=[CH:4][N:3]=1.C(OCC)(=O)C>Cl>[NH2:24][CH:17]([C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)[C:16]([N:13]1[CH2:14][CH2:15][CH:10]([N:8]2[CH2:9][C:5]3=[CH:4][N:3]=[C:2]([CH3:1])[N:6]3[C:7]2=[O:33])[CH2:11][CH2:12]1)=[O:32]
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 8857Ethyl AcetateHCID 23138346tert-butyl 2-(4-(5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)-1-piperidinyl)-2-oxo-1-phenylethylcarbamate

生成物 1

HCID 231380962-(1-(2-amino-2-phenylacetyl)-4-piperidinyl)-5-methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one収率 31%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

tert-Butyl 2-(4-(5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)-1-piperidinyl)-2-oxo-1-phenylethylcarbamate (0.43 g) obtained in Example 50a) was dissolved in concentrated hydrochloric acid (1.5 ml), and mixed at room temperature for 5 minutes. Ethyl acetate was added thereto, and the reaction mixture was washed with an aqueous sodium hydrogen carbonate solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound as colorless powder (0.10 g, 31%).

後処理

  1. additionmixed at room temperature for 5 minutes
  2. washthe reaction mixture was washed with an aqueous sodium hydrogen carbonate solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-a95b1b19816c4872abd5fbee45f0afaa
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07820673B2

反応ノート

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