HCID 178499149、化合物 → Methyl 7-benzyl-5,6,7,8-tetrahydroimidazo[1,5-a]pyrazine-1-carboxylate

HRID 1808349ノート

反応式

HRID 1808349 の反応式
[CH2:1]([N:8]([CH2:12][C:13]1[N:14]=[CH:15][NH:16][C:17]=1[C:18]([O:20][CH3:21])=[O:19])[CH2:9][CH2:10]Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(#N)C>[CH2:1]([N:8]1[CH2:9][CH2:10][N:14]2[CH:15]=[N:16][C:17]([C:18]([O:20][CH3:21])=[O:19])=[C:13]2[CH2:12]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

3

反応物 1

HCID 178499149HCID 178499149、化合物

生成物 1

HCID 57635262Methyl 7-benzyl-5,6,7,8-tetrahydroimidazo[1,5-a]pyrazine-1-carboxylate収率 64%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

TEA (28.66 mmol, 4 equiv.) was added at 0° C. to a solution of methyl 4-((benzyl(2-chloroethyl)amino)methyl)-1H-imidazole-5-carboxylate (7.16 mmol, 1 equiv.) in acetonitrile (50 ml). The resulting mixture was heated for 16 h at 80° C. It was then cooled and filtered, and the filtrate was concentrated in vacuo. The crude product was taken up in DCM and sat. sodium hydrogen carbonate solution, and the organic phase was dried and concentrated in vacuo. The resulting crude product was purified by column chromatography (silica gel, 5% MeOH in DCM), and the desired product was thus obtained in the form of a brown solid. Yield: 64%

後処理

  1. temperatureIt was then cooled
  2. filtrationfiltered
  3. concentrationthe filtrate was concentrated in vacuo
  4. dry with materialsat. sodium hydrogen carbonate solution, and the organic phase was dried
  5. concentrationconcentrated in vacuo
  6. customThe resulting crude product was purified by column chromatography (silica gel, 5% MeOH in DCM)

出典と根拠

ORDレコード
ord-4a6b0c6c89a340e8846055e876062f55
出典データセット
uspto-grants-2013_01
特許番号
US08357717B2

反応ノート

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