Sodium Iodide → [5-(2-Fluoro-phenyl)-1-methyl-2,3-dihydro-1H-benzo[e][1,4]diazepin-2-ylmethyl]-(3-trifluoromethyl-phenyl)-amine

HRID 1591258

反応式

HRID 1591258 の反応式
[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C:6]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[F:19])=[N:5][CH2:4][CH:3]1[CH2:20]Cl.[F:22][C:23]([F:32])([F:31])[C:24]1[CH:25]=[C:26]([CH:28]=[CH:29][CH:30]=1)[NH2:27].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C)C=O>[CH3:1][N:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C:6]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[F:19])=[N:5][CH2:4][CH:3]1[CH2:20][NH:27][C:26]1[CH:28]=[CH:29][CH:30]=[C:24]([C:23]([F:22])([F:31])[F:32])[CH:25]=1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 73753-(Trifluoromethyl)anilineHCID 11430Potassium CarbonateHCID 134856441-methyl-2-chloromethyl-5-(2'-fluorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine

生成物 1

HCID 19766234[5-(2-Fluoro-phenyl)-1-methyl-2,3-dihydro-1H-benzo[e][1,4]diazepin-2-ylmethyl]-(3-trifluoromethyl-phenyl)-amine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

According to the method of Example 5, 1-methyl-2-chloromethyl-5-(2'-fluorophenyl)-2,3-dihydro-1H-1,4-benzodiazepine (200 mg, 0.66 mmole) and m-trifluoromethyl aniline (319 mg, 1.97 mmole) were combined in 2 ml of dry N,N-dimethylformamide, and potassium carbonate (273 mg, 1.97 mmole) and sodium iodide (198 mg, 1.32 mmole) were added to this mixture (which was heated at 65° C. for 18 hours). After solvent-removal, partitioning, separation, washing, drying and concentrating, the analytical product was obtained via chromatography on silica gel (ethyl acetate-hexane elution, 3:7 v/v) and was shown to be 96% pure by HPLC.

後処理

  1. customAfter solvent-removal
  2. custompartitioning
  3. customseparation
  4. washwashing
  5. customdrying
  6. concentrationconcentrating
  7. customthe analytical product was obtained via chromatography on silica gel (ethyl acetate-hexane elution, 3:7 v/v)

出典と根拠

ORDレコード
ord-d3633dff796e438999bca76019025104
出典データセット
uspto-grants-1993_04
特許番号
US05206238

関連ノート

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