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

HRID 1162295ノート

反応式

HRID 1162295 の反応式
CC(O[C:6]([NH:8][C@@H:9]([C:16](O)=O)[C:10]1[CH:15]=CC=CC=1)=[O:7])(C)C.C1C=C[C:22]2[N:27](O)N=[N:25][C:23]=2[CH:24]=1.C[CH2:30][N:31]=C=NCCCN(C)C.[CH2:40](N(CC)CC)[CH3:41]>C(#N)C>[CH3:40][C:41]1[N:25]2[C:6](=[O:7])[N:8]([CH:9]3[CH2:10][CH2:15][NH:31][CH2:30][CH2:16]3)[CH2:24][C:23]2=[CH:22][N:27]=1

参加物

6

反応物 4

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 2755953(2R)-2-{[(tert-butoxy)carbonyl]amino}-2-phenylacetic acid

生成物 1

HCID 230840155-methyl-2-(4-piperidinyl)-1,2-dihydro-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 Boc-D-phenylglycine (1.3 g) and HOBt (1.2 g) in acetonitrile (30 ml) was added WSC (1.4 g), and the reaction mixture was mixed at room temperature for 15 minutes. Then, 5-methyl-2-(4-piperidinyl)-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one (1.1 g) obtained in Reference Example 1 and triethylamine (2.1 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 silica gel column (ethyl acetate to ethyl acetate/methanol=10/1) to obtain the title compound as colorless powder (2.1 g, 93%).

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-4a1169b5086b46619cc0a4181c022a90
出典データセット
uspto-grants-2010_10
特許番号
US07820673B2

反応ノート

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