Water → 2-(2-(4-Methoxycarbonylphenylmethyl)aminonitrobenzen-5-yl)benzoxazole

HRID 74297

반응식

HRID 74297 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(N(CC)CC)C.Cl.[C:28]([C:32]1[CH:39]=[CH:38][C:35]([CH2:36][NH2:37])=[CH:34][CH:33]=1)([O:30][CH3:31])=[O:29].O>C(#N)C>[CH3:31][O:30][C:28]([C:32]1[CH:39]=[CH:38][C:35]([CH2:36][NH:37][C:2]2[CH:7]=[CH:6][C:5]([C:8]3[O:9][C:10]4[CH:16]=[CH:15][CH:14]=[CH:13][C:11]=4[N:12]=3)=[CH:4][C:3]=2[N+:17]([O-:19])=[O:18])=[CH:34][CH:33]=1)=[O:29]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 2729253Methyl 4-(aminomethyl)benzoate hydrochlorideHCID 219909702-(4-Fluoro-3-nitrophenyl)benzoxazole

생성물 1

HCID 674984512-(2-(4-Methoxycarbonylphenylmethyl)aminonitrobenzen-5-yl)benzoxazole수율 95.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a suspension of 2-(4-fluoro-3-nitrophenyl)benzoxazole (see Working Example 15-2) (250 mg, 0.968 mmol) in acetonitrile (5 mL) was added triethylamine (245 mg, 2.42 mmol) and 4-carbomethoxybenzylamine hydrochloride (215 mg, 1.07 mmol), and this was heated to reflux for 2 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 (372 mg, 95% yield).

후처리

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

출처 및 근거

ORD 기록
ord-4edf92dcebf1480ca969c2aa9d0f382b
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

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