9-(3-Fluorobiphenyl-4-yl)-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide → 9-(3-Fluorobiphenyl-4-yl)-3,4,6,7,8,9-hexahydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide
反応式
[F:1][C:2]1[CH:3]=[C:4]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:5]=[CH:6][C:7]=1[C:8]1[C:13]2=[N:14][S:15](=[O:19])(=[O:18])[CH2:16][CH2:17][N:12]2[CH:11]=[CH:10][CH:9]=1>C1COCC1.CO.[C].[Pd].[C].[Rh]>[F:1][C:2]1[CH:3]=[C:4]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:5]=[CH:6][C:7]=1[CH:8]1[C:13]2=[N:14][S:15](=[O:19])(=[O:18])[CH2:16][CH2:17][N:12]2[CH2:11][CH2:10][CH2:9]1参加物
5
反応物 1
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 50 °C
実験手順
To a solution of 9-(3-fluorobiphenyl-4-yl)-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide (200 mg) in THF/methanol (30 mL/30 mL) was added 10% palladium carbon (50 mg). The reaction mixture was stirred under a hydrogen atmosphere at 50° C. for 1 day. 5% Rhodium carbon (100 mg) was added, and the reaction mixture was stirred under a hydrogen atmosphere at room temperature for 7 hr, and insoluble material was filtered off through celite. The filtrate was concentrated under reduced pressure, and the obtained residue was purified by recrystallization (methanol-THF/diisopropyl ether) to give the title compound (154.4 mg).
後処理
- stirringthe reaction mixture was stirred under a hydrogen atmosphere at room temperature for 7 hr
- filtrationinsoluble material was filtered off through celite
- concentrationThe filtrate was concentrated under reduced pressure
- customthe obtained residue was purified by recrystallization (methanol-THF/diisopropyl ether)
出典と根拠
- ORDレコード
- ord-768f8f5894fa42a19c62111864b493b3
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08916551B2
反応ノート
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