Phosphorus oxychloride → HCID 178526406、化合物

HRID 1521359ノート

反応式

HRID 1521359 の反応式
[Cl:1][C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:5]2[NH:6][C:7](=O)[NH:8][C:4]=2[CH:3]=1.P(Cl)(Cl)([Cl:17])=O>>[Cl:17][C:7]1[NH:8][C:4]2[CH:3]=[C:2]([Cl:1])[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:5]=2[N:6]=1

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 145662265-Chloro-1,3-dihydro-6-nitro-2H-benzimidazol-2-one

生成物 1

HCID 178526406HCID 178526406、化合物収率 89%

反応条件

温度
85 °C

実験手順

To 5-chloro-6-nitro-1,3-dihydro-benzoimidazol-2-one (5.63 g, 26.35 mmol) was added phosphorus oxychloride (35 mL) and the reaction mixture was heated to 85° C. for 36 h. The reaction mixture was concentrated and the residue triturated with cold saturated aqueous sodium bicarbonate (to pH 8, 0.8 L). The resulting precipitate was collected and dried to yield the titled compound (5.43 g, 89% yield). MS (ESI/CI): mass calcd. for C7H3Cl2N3O2, 231.0; m/z found, 232.0 [M+H]+.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. customthe residue triturated with cold saturated aqueous sodium bicarbonate (to pH 8, 0.8 L)
  3. customThe resulting precipitate was collected
  4. customdried

出典と根拠

ORDレコード
ord-b796a6adb6a84f0d9bc8c842c0342adf
出典データセット
uspto-grants-2015_07
特許番号
US09073923B2

反応ノート

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