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

HRID 1349479노트

반응식

HRID 1349479 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
90 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d4cbc04d18734d5d81fbcb2ad98194d6
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211572B2

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