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Water → HCID 67380925、化合物

HRID 1804269
ノート
印刷プレビュー

反応式

HRID 1804269 の反応式
[CH3:1][C@@H:2]1[CH2:6][O:5][C:4](=[O:7])[NH:3]1.[H-].[Na+].[Br:10][C:11]1[CH:12]=[C:13]([CH3:33])[C:14]([N:17]2[CH2:22][CH2:21][N:20]([C:23]([C:25]3[CH:26]=[N:27][C:28](F)=[CH:29][C:30]=3[CH3:31])=[O:24])[CH2:19][CH2:18]2)=[N:15][CH:16]=1.O>CN(C=O)C>[Br:10][C:11]1[CH:12]=[C:13]([CH3:33])[C:14]([N:17]2[CH2:18][CH2:19][N:20]([C:23]([C:25]3[C:30]([CH3:31])=[CH:29][C:28]([N:3]4[C@H:2]([CH3:1])[CH2:6][O:5][C:4]4=[O:7])=[N:27][CH:26]=3)=[O:24])[CH2:21][CH2:22]2)=[N:15][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 2734858(R)-4-Methyloxazolidin-2-oneHCID 58484740HCID 58484740、化合物

生成物 1

HCID 67380925HCID 67380925、化合物収率 48.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of (R)-4-methyloxazolidin-2-one (222 mg) described in Preparation Example 25 in DMF (4 mL) was added sodium hydride (84 mg) at 10° C., and the mixture was stirred for 30 min. Furthermore, [4-(5-bromo-3-methylpyridin-2-yl)piperazin-1-yl](6-fluoro-4-methylpyridin-3-yl)methanone (447 mg) described in Preparation Example 113 was added, and the mixture was stirred at 80° C. for 3 hr and at 100° C. for 3 hr. After cooling, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and the solvent was evaporated. The residue was purified by column chromatography (hexane:ethyl acetate) to give (R)-3-{5-[4-(5-bromo-3-methylpyridin-2-yl)piperazine-1-carbonyl]-4-methylpyridin-2-yl}-4-methyloxazolidin-2-one (260 mg).

後処理

  1. additionwas added
  2. stirringthe mixture was stirred at 80° C. for 3 hr and at 100° C. for 3 hr
  3. temperatureAfter cooling
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. customthe solvent was evaporated
  7. customThe residue was purified by column chromatography (hexane:ethyl acetate)

出典と根拠

ORDレコード
ord-812136c024ac4a65a095d88089ef4ad7
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08354401B2

反応ノート

読み込み中…

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