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

HRID 1162328
ノート
印刷プレビュー

反応式

HRID 1162328 の反応式
[CH3:1][C:2]1[N:6]2[C:7](=[O:24])[N:8]([CH2:10][CH:11]3[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]3)[CH2:9][C:5]2=[CH:4][N:3]=1.[ClH:25]>C(O)C>[ClH:25].[ClH:25].[CH3:1][C:2]1[N:6]2[C:7](=[O:24])[N:8]([CH2:10][CH:11]3[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]3)[CH2:9][C:5]2=[CH:4][N:3]=1
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 313Hydrochloric AcidHCID 23138425tert-butyl 4-((5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)methyl)-1-piperidinecarboxylate

生成物 1

HCID 231381375-methyl-2-(4-piperidinyl)methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride収率 78%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To tert-butyl 4-((5-methyl-3-oxo-1H-imidazo[1,5-c]imidazol-2(3H)-yl)methyl)-1-piperidinecarboxylate (3.5 g) obtained in Example 85a) was added concentrated hydrochloric acid (10 ml), and mixed for 10 minutes. To the reaction mixture was added ethanol, and the solvent was distilled off under reduced pressure. To the residue was further added ethanol, and the solvent was distilled off under reduced pressure. To the residue was added isopropyl alcohol, and the precipitate was collected by filtration. The precipitate was washed sequentially with isopropyl alcohol and diethyl ether and dried under reduced pressure to obtain 5-methyl-2-(4-piperidinyl)methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride as a colorless solid (2.5 g, 78%).

後処理

  1. additionmixed for 10 minutes
  2. distillationthe solvent was distilled off under reduced pressure
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionTo the residue was added isopropyl alcohol
  5. filtrationthe precipitate was collected by filtration
  6. washThe precipitate was washed sequentially with isopropyl alcohol and diethyl ether
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-3c01014afba649549ba72d67538716f5
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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