Phosphorus oxychloride → HCID 178526406, 화합물

HRID 408687노트

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HRID 408687 반응식
[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

참가 물질

3

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

생성물 1

HCID 178526406HCID 178526406, 화합물수율 89%

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온도
85 °C

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-7972eab6a400499189cb153507702d8c
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08759345B2

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