反応式
N[C:2]1[CH:12]=[CH:11][C:10]2[CH:9]3[CH2:13][CH:5]([CH2:6][N:7]([C:14](=[O:19])[C:15]([F:18])([F:17])[F:16])[CH2:8]3)[C:4]=2[CH:3]=1.N([O-])=O.[Na+].[ClH:24]>O.Cl[Cu]>[Cl:24][C:2]1[CH:12]=[CH:11][C:10]2[CH:9]3[CH2:13][CH:5]([CH2:6][N:7]([C:14](=[O:19])[C:15]([F:18])([F:17])[F:16])[CH2:8]3)[C:4]=2[CH:3]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 60 °C
実験手順
1-(4-Amino-10-aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-2,2,2-trifluoro-ethanone (460 mg, 1.7 mmol) was dissolved in H2O (2 mL) and concentrated HCl solution(1 mL) then cooled to 0° C. and treated with a solution of sodium nitrite (NaNO2) (275 mg) in H2O (1 mL) dropwise. To the resulting solution was added a CuCl (202 mg, prepared as described above, 2.04 mmol) in concentrated HCl solution (2 mL) over 10 minutes (gas evolution observed). The resulting solution was warmed to 60° C. for 15 minutes, then was cooled to room temperature and extracted with ethyl acetate (4×30 mL). After drying over Na2SO4, the solution was filtered and concentrated to an oil which was filtered through a Silica pad to remove baseline material eluting with 50% ethyl acetate/hexanes to give an oil (470 mg, 95%).
後処理
- temperaturewas cooled to room temperature
- extractionextracted with ethyl acetate (4×30 mL)
- dry with materialAfter drying over Na2SO4
- filtrationthe solution was filtered
- concentrationconcentrated to an oil which
- filtrationwas filtered through a Silica pad
- customto remove baseline material
- washeluting with 50% ethyl acetate/hexanes
出典と根拠
- ORDレコード
- ord-a0e1cb1ebb244b41a71131589d967acf
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091372B2
関連ノート
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