Acetonitrile → 6-(5-Bromo-2-fluorophenyl)-N-(2-(2-fluorophenyl)propan-2-yl)-1,2,4-triazin-3-amine

HRID 2276770ノート

反応式

HRID 2276770 の反応式
Br[C:2]1[N:3]=[N:4][C:5]([C:8]2[CH:13]=[C:12]([Br:14])[CH:11]=[CH:10][C:9]=2[F:15])=[CH:6][N:7]=1.[F:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[C:23]([NH2:26])([CH3:25])[CH3:24].C([O-])([O-])=O.[K+].[K+].CC#N>CCOC(C)=O>[Br:14][C:12]1[CH:11]=[CH:10][C:9]([F:15])=[C:8]([C:5]2[N:4]=[N:3][C:2]([NH:26][C:23]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=3[F:16])([CH3:25])[CH3:24])=[N:7][CH:6]=2)[CH:13]=1

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 135695202-(2-Fluorophenyl)propan-2-amineHCID 866868233-Bromo-6-(5-bromo-2-fluorophenyl)-1,2,4-triazine

生成物 1

HCID 866868246-(5-Bromo-2-fluorophenyl)-N-(2-(2-fluorophenyl)propan-2-yl)-1,2,4-triazin-3-amine収率 67.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

3-Bromo-6-(5-bromo-2-fluorophenyl)-1,2,4-triazine (2.8 g, 8.4 mmol), 2-(2-fluorophenyl)propan-2-amine (2.0 g, 12.6 mmol), K2CO3 (2.3 g, 16.8 mmol) and CH3CN (20 mL) was heated to 90° C. The reaction mixture was diluted with EtOAc and washed with satd. aq. NaHCO3 and brine. The organic layer was dried over sodium sulfate, filtered, concentrated, and purified using silica gel chromatography to afford a yellow solid (2.3 g), m/z=406.1 [M+H].

後処理

  1. washwashed with satd
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. custompurified

出典と根拠

ORDレコード
ord-b3bb45e774414efeb5124266787b9838
出典データセット
uspto-grants-2015_09
特許番号
US09133123B2

反応ノート

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