Dimethylformamide → HCID 178505514、化合物

HRID 594928ノート

反応式

HRID 594928 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[NH:16][C:11]2=[CH:12][N:13]=[CH:14][CH:15]=[C:10]2[CH:9]=1.[OH-:17].[Na+].Cl[CH2:20][C:21]1[O:25][N:24]=[C:23]([C:26]2[CH:31]=[CH:30][C:29]([F:32])=[CH:28][C:27]=2[C:33]([F:36])([F:35])[F:34])[CH:22]=1.CN([CH:40]=[O:41])C>>[F:34][C:33]([F:36])([F:35])[C:40]([O-:41])=[O:17].[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:9]=[C:10]2[CH:15]=[CH:14][N:13]([CH2:20][C:21]3[O:25][N:24]=[C:23]([C:26]4[CH:31]=[CH:30][C:29]([F:32])=[CH:28][C:27]=4[C:33]([F:36])([F:34])[F:35])[CH:22]=3)[CH:12]=[C:11]2[NH+:16]=1

参加物

5

反応物 4

HCID 6228Dimethylformamide2 回HCID 14798Sodium HydroxideHCID 468639965-Chloromethyl-3-(4-fluoro-2-trifluoromethyl-phenyl)-isoxazoleHCID 574382742-(2-Fluoro-phenyl)-1H-pyrrolo[2,3-c]pyridine

生成物 1

HCID 178505514HCID 178505514、化合物収率 81%

実験手順

To a solution of 2-(2-Fluoro-phenyl)-1H-pyrrolo[2,3-c]pyridine (50 mg, 0.244 mmole) in DMF (1 ml) was added 10% (w/v) aqueous NaOH (113 μl, 0.28 mmole) followed by a solution of 5-Chloromethyl-3-(4-fluoro-2-trifluoromethyl-phenyl)-isoxazole (79 mg, 0.28 mmole) in DMF (0.5 ml). The reaction mixture was stirred at room temperature for 12 hours. The crude reaction mixture was purified by reverse phase HPLC with mass directed collection. Obtained 109 mg (81%) of 2-(2-Fluoro-phenyl)-6-[3-(4-fluoro-2-trifluoromethyl-phenyl)-isoxazol-5-ylmethyl]-6H-pyrrolo[2,3-c]pyridinium trifluoroacetate.

後処理

  1. customThe crude reaction mixture
  2. customwas purified by reverse phase HPLC with mass
  3. customcollection

出典と根拠

ORDレコード
ord-6c385806003140f5a7735905b553d23d
出典データセット
uspto-grants-2016_01
特許番号
US09242983B2

反応ノート

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