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

HRID 74312

반응식

HRID 74312 반응식
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]

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 87697(2-(Methylthio)ethyl)amineHCID 219909702-(4-Fluoro-3-nitrophenyl)benzoxazole

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e56c8d56a3744d859bc7775f1186abe7
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

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