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Triethylamine → 1,2-Dihydro-5-methyl-2-(1-piperazinyl)-3H-imidazo[1,5-c]imidazol-3-one

HRID 1162300
ノート
印刷プレビュー

反応式

HRID 1162300 の反応式
[C:1]([O:5]C(NC(C(CC)(O)CC)C(O)=O)=O)(C)(C)C.C1C=C[C:22]2[N:27](O)[N:26]=[N:25][C:23]=2[CH:24]=1.[CH3:29][CH2:30][N:31]=C=NCCCN(C)C.C([N:42]([CH2:45][CH3:46])[CH2:43][CH3:44])C>C(#N)C>[CH3:29][C:30]1[N:25]2[C:1](=[O:5])[N:27]([N:26]3[CH2:44][CH2:43][NH:42][CH2:45][CH2:46]3)[CH2:22][C:23]2=[CH:24][N:31]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 23138330HCID 23138330、化合物

生成物 1

HCID 231384181,2-Dihydro-5-methyl-2-(1-piperazinyl)-3H-imidazo[1,5-c]imidazol-3-one

試薬・触媒・溶媒 1

HCID 6342Acetonitrile
溶媒

実験手順

To a solution of 2-((tert-butoxycarbonyl)amino)-3-ethyl-3-hydroxypentanoic acid (0.80 g) obtained in Example 36b) and HOBt (0.65 g) in acetonitrile (30 ml) was added WSC (0.83 g), and the reaction mixture was mixed at room temperature for 15 minutes. Then, 5-methyl-2-(1-piperazinyl)-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one (0.63 g) obtained in Reference Example 2 and triethylamine (1.2 ml) were added thereto. The reaction mixture was mixed at room temperature for 15 hours, the solvent was then distilled off under reduced pressure, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with an aqueous sodium hydrogen carbonate solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified with basic silica gel column (ethyl acetate) to obtain the title compound as colorless powder (0.11 g, 8%).

後処理

  1. additionthe reaction mixture was mixed at room temperature for 15 minutes

出典と根拠

ORDレコード
ord-b9c161d8e5044e7fbc6d37465287313e
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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