9-benzyloxy-2-(3-chlorobenzyl)-7-(2,2-dimethylbutyryl)-3,4-dihydro-2H-pyrido[1,2-a]pyrazine-1,8-dione → 2-[(3-Chlorophenyl)methyl]-7-(2,2-dimethylbutanoyl)-9-hydroxy-3,4-dihydropyrido[1,2-a]pyrazine-1,8-dione

HRID 1349500노트

반응식

HRID 1349500 반응식
C([O:8][C:9]1[C:10](=[O:35])[C:11]([C:28](=[O:34])[C:29]([CH3:33])([CH3:32])[CH2:30][CH3:31])=[CH:12][N:13]2[CH2:18][CH2:17][N:16]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=3)[C:15](=[O:27])[C:14]=12)C1C=CC=CC=1>FC(F)(F)C(O)=O>[Cl:26][C:22]1[CH:21]=[C:20]([CH:25]=[CH:24][CH:23]=1)[CH2:19][N:16]1[CH2:17][CH2:18][N:13]2[CH:12]=[C:11]([C:28](=[O:34])[C:29]([CH3:32])([CH3:33])[CH2:30][CH3:31])[C:10](=[O:35])[C:9]([OH:8])=[C:14]2[C:15]1=[O:27]

참가 물질

3

반응물 1

HCID 230774849-benzyloxy-2-(3-chlorobenzyl)-7-(2,2-dimethylbutyryl)-3,4-dihydro-2H-pyrido[1,2-a]pyrazine-1,8-dione

생성물 1

HCID 546833552-[(3-Chlorophenyl)methyl]-7-(2,2-dimethylbutanoyl)-9-hydroxy-3,4-dihydropyrido[1,2-a]pyrazine-1,8-dione수율 71.2%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

9-Benzyloxy-2-(3-chlorobenzyl)-7-(2,2-dimethylbutyryl)-3,4-dihydro-2H-pyrido[1,2-a]pyrazine-1,8-dione (55 mg) was dissolved in trifluoroacetic acid (0.5 ml) and the mixture was stirred at room temperature for 30 min. The solvent was evaporated and toluene was added, and the mixture was concentrated, which operations were performed twice. Crystallization from chloroform-diisopropyl ether gave 2-(3-chlorobenzyl)-7-(2,2-dimethylbutyryl)-9-hydroxy-3,4-dihydro-2H-pyrido[1,2-a]pyrazine-1,8-dione (32 mg).

후처리

  1. customThe solvent was evaporated
  2. additiontoluene was added
  3. concentrationthe mixture was concentrated
  4. customCrystallization from chloroform-diisopropyl ether

출처 및 근거

ORD 기록
ord-1bfa144d9ff14d4d84e815ae5f37897e
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211572B2

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