Water → N-(2-(methylthio)ethyl)-4-(benzoxazol-2-yl)-2-nitroaniline

HRID 74312

反応式

HRID 74312 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][S:27][CH2:28][CH2:29][NH2:30].O>C(#N)C>[CH3:26][S:27][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 87697(2-(Methylthio)ethyl)amineHCID 219909702-(4-Fluoro-3-nitrophenyl)benzoxazole

生成物 1

HCID 67498515N-(2-(methylthio)ethyl)-4-(benzoxazol-2-yl)-2-nitroaniline収率 98%

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) (300 mg, 1.16 mmol) in acetonitrile (5 mL) was added potassium carbonate (321 mg, 1.55 mmol) and 2-(methylthio)ethylamine (127 mg, 1.39 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 (373 mg, 98% yield) as red 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-e56c8d56a3744d859bc7775f1186abe7
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

関連ノート

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