Hydrochloric Acid → 2-(3-chlorobenzyl)-9-hydroxy-7-phenyl-2H-pyrido[1,2-a]pyrazine-1,8-dione hydrochloride

HRID 1349479ノート

反応式

HRID 1349479 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:36]=[CH:37][CH:38]=1)[CH2:5][NH:6][C:7]([C:9]1[N:10]([CH2:30][CH:31](OC)OC)[CH:11]=[C:12]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:13](=[O:23])[C:14]=1[O:15]CC1C=CC=CC=1)=[O:8].Cl>C(O)(=O)C>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH:36]=[CH:37][CH:38]=1)[CH2:5][N:6]1[CH:31]=[CH:30][N:10]2[CH:11]=[C:12]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[C:13](=[O:23])[C:14]([OH:15])=[C:9]2[C:7]1=[O:8]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 588591413-Benzyloxy-1-(2,2-dimethoxyethyl)-4-oxo-5-phenyl-1,4-dihydropyridine-2-carboxylic acid 3-chlorobenzylamide

生成物 1

HCID 547054042-(3-chlorobenzyl)-9-hydroxy-7-phenyl-2H-pyrido[1,2-a]pyrazine-1,8-dione hydrochloride収率 192.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

3-Benzyloxy-1-(2,2-dimethoxyethyl)-4-oxo-5-phenyl-1,4-dihydropyridine-2-carboxylic acid 3-chlorobenzylamide (52 mg) was dissolved in acetic acid (0.5 ml) and conc. hydrochloric acid (0.5 ml) was added, and the mixture was stirred at 90° C. for 2 hr. The reaction mixture was concentrated, toluene was added to the residue and the mixture was concentrated, which operations were performed twice. Methanol was further added and the mixture was concentrated and crystallized from ethyl acetate-diisopropyl ether to give 2-(3-chlorobenzyl)-9-hydroxy-7-phenyl-2H-pyrido[1,2-a]pyrazine-1,8-dione hydrochloride (39 mg).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additiontoluene was added to the residue
  3. concentrationthe mixture was concentrated
  4. additionMethanol was further added
  5. concentrationthe mixture was concentrated
  6. customcrystallized from ethyl acetate-diisopropyl ether

出典と根拠

ORDレコード
ord-d4cbc04d18734d5d81fbcb2ad98194d6
出典データセット
uspto-grants-2007_05
特許番号
US07211572B2

反応ノート

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