Sodium Bicarbonate → HCID 58012362, 화합물

HRID 1698545노트

반응식

HRID 1698545 반응식
Cl[C:2]1[N:6]([CH3:7])[C:5]2[C:8]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH2:18][CH3:19])=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]=1.[Br:20][C:21]1[CH:27]=[C:26]([CH3:28])[C:24]([NH2:25])=[C:23]([O:29][CH3:30])[CH:22]=1.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[Br:20][C:21]1[CH:27]=[C:26]([CH3:28])[C:24]([NH:25][C:2]2[N:6]([CH3:7])[C:5]3[C:8]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=4[CH2:18][CH3:19])=[CH:9][CH:10]=[CH:11][C:4]=3[N:3]=2)=[C:23]([O:29][CH3:30])[CH:22]=1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 106802184-Bromo-2-methoxy-6-methylanilineHCID 67273043HCID 67273043, 화합물

생성물 1

HCID 58012362HCID 58012362, 화합물수율 54.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

A mixture of 100 mg (0.369 mmol) of 2-chloro-7-(2-ethylphenyl)-1-methyl-1H-benzimidazole and 239 mg (1.11 mmol) of 4-bromo-2-methoxy-6-methylaniline was stirred at 120° C. for 15 hours. After cooling, the reaction mixture was neutralized by saturated aqueous sodium hydrogen carbonate, followed by addition of ethyl acetate. The resulting crystals were collected by filtration and washed with water and ethyl acetate, and suspended in hot ethyl acetate. After cooling to room temperature, the crystals were collected by filtration and washed with ethyl acetate and a 50% dimethylsulfoxide/methanol mixture to give 90 mg (54%) of the title compound.

후처리

  1. temperatureAfter cooling
  2. filtrationThe resulting crystals were collected by filtration
  3. washwashed with water and ethyl acetate
  4. temperatureAfter cooling to room temperature
  5. filtrationthe crystals were collected by filtration
  6. washwashed with ethyl acetate

출처 및 근거

ORD 기록
ord-28918a6c8bc64e0488f7d7a2fd6b6f38
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08163935B2

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