Phosphorus oxychloride → Methyl 2,4-dichloro-1-methyl-1H-benzimidazole-7-carboxylate

HRID 1698577노트

반응식

HRID 1698577 반응식
[Cl:1][C:2]1[C:7]2[NH:8][C:9](=O)[N:10]([CH3:11])[C:6]=2[C:5]([C:13]([O:15][CH3:16])=[O:14])=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:19])=O>C(OCC)(=O)C>[Cl:19][C:9]1[N:10]([CH3:11])[C:6]2[C:5]([C:13]([O:15][CH3:16])=[O:14])=[CH:4][CH:3]=[C:2]([Cl:1])[C:7]=2[N:8]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 67272570Methyl 7-chloro-3-methyl-2-oxo-2,3-dihydro-1H-benzimidazole-4-carboxylate

생성물 1

HCID 67272934Methyl 2,4-dichloro-1-methyl-1H-benzimidazole-7-carboxylate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
110 °C

실험 절차

Methyl 7-chloro-3-methyl-2-oxo-2,3-dihydro-1H-benzimidazole-4-carboxylate (150 mg, 0.63 mmol) was dissolved in 3 mL of phosphorous oxychloride and heated at 110° C. overnight. The reaction mixture was allowed to cool to room temperature, poured into a crushed ice, and stirred for 1 h. The resultant was diluted in ethyl acetate, washed with aqueous sodium bicarbonate, dried over magnesium sulfate, filtered and concentrated in vacuo. The obtained (147 mg, 90%) was used in the next reaction without further purification.

후처리

  1. temperatureto cool to room temperature
  2. washwashed with aqueous sodium bicarbonate
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe obtained (147 mg, 90%)
  7. customwas used in the next reaction without further purification

출처 및 근거

ORD 기록
ord-298015aa55ab4d9d9d04662326f52a58
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163935B2

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