Water → N-(2-dimethylaminoethyl)-4-(benzoxazol-2-yl)-2-nitroaniline

HRID 74311ノート

反応式

HRID 74311 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:4][C:3]=1[N+:17]([O-:19])=[O:18].C(=O)([O-])[O-].[K+].[K+].[CH3:26][N:27]([CH3:31])[CH2:28][CH2:29][NH2:30].O>C(#N)C>[CH3:26][N:27]([CH3:31])[CH2:28][CH2:29][NH:30][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][C:10]3[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:4][C:3]=1[N+:17]([O-:19])=[O:18]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 66053N,N-DimethylethylenediamineHCID 219909702-(4-Fluoro-3-nitrophenyl)benzoxazole

生成物 1

HCID 67498833N-(2-dimethylaminoethyl)-4-(benzoxazol-2-yl)-2-nitroaniline収率 95%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a suspension of 2-(4-fluoro-3-nitrophenyl)benzoxazole (see Working Example 15-2) (200 mg, 0.775 mmol) in acetonitrile (5 mL) was added potassium carbonate (214 mg, 1.55 mmol) and N,N-dimethylethylenediamine (82 mg, 0.93 mmol), and this was heated to reflux for 3 hours. After the reaction was complete, this was cooled to room temperature, water was added, and after the precipitated crystals were filtered and washed with water, they were dried to yield the title compound (240 mg, 95% yield) as orange crystals.

後処理

  1. temperaturethis was heated
  2. temperatureto reflux for 3 hours
  3. filtrationafter the precipitated crystals were filtered
  4. washwashed with water, they
  5. customwere dried

出典と根拠

ORDレコード
ord-f0548328b9ba49da8773e3c330c166e1
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

反応ノート

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