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

HRID 74297

反応式

HRID 74297 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(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]

参加物

6

反応物 4

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

生成物 1

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

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) (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).

後処理

  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

出典と根拠

ORDレコード
ord-4edf92dcebf1480ca969c2aa9d0f382b
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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