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

HRID 1162358
ノート
印刷プレビュー

反応式

HRID 1162358 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.[ClH:34]>C(O)C>[ClH:34].[ClH:34].[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 313Hydrochloric AcidHCID 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 231383382-(1-(2-amino-2-phenylacetyl)-4-piperidinyl)-5-methyl-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol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 (13 g) obtained in Example 50a) was dissolved in concentrated hydrochloric acid (30 ml) and ethanol (30 ml). The reaction mixture was mixed at room temperature for 30 minutes, and then the solvent was distilled off under reduced pressure. Water in the residue was removed by azeotropy with ethanol to obtain the title compound as pale yellow powder (12 g, quantitative).

後処理

  1. additionThe reaction mixture was mixed at room temperature for 30 minutes
  2. distillationthe solvent was distilled off under reduced pressure
  3. customWater in the residue was removed by azeotropy with ethanol

出典と根拠

ORDレコード
ord-f32132efc5eb41a2a372e6bb24d4dd36
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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