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 1349500ノート

反応式

HRID 1349500 の反応式
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]

参加物

3

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-1bfa144d9ff14d4d84e815ae5f37897e
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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