Water → 5,6-difluoro-1H-1,3-benzodiazol-2-amine

HRID 415124

반응식

HRID 415124 반응식
[F:1][C:2]1[CH:3]=[C:4]([NH2:10])[C:5]([NH2:9])=[CH:6][C:7]=1[F:8].O.[N:12]#[C:13]Br.C(=O)([O-])O.[Na+]>C(#N)C>[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]2[NH:9][C:13]([NH2:12])=[N:10][C:4]=2[CH:3]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 10476Cyanogen BromideHCID 516892Sodium BicarbonateHCID 27367551,2-Diamino-4,5-difluorobenzene

생성물 1

HCID 106787085,6-difluoro-1H-1,3-benzodiazol-2-amine수율 40%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

4,5-Difluorobenzene-1,2-diamine (0.651 g, 0.562 mmol, commercially available from Matrix Scientific) in acetonitrile (10 mL) and water (2 ml) at 0° C. was treated with cyanogen bromide (0.063 g, 0.6 mmol). The reaction mixture was allowed to warm to room temperature, and then stirred for 14 hours. The reaction mixture was then treated with saturated aqueous sodium hydrogen carbonate solution (50 ml) and shaken. The resulting solid was filtered off, washed with water and dried under reduced pressure to give 0.39 g of 5,6-difluoro-1H-benzo[d]imidazol-2-amine (yield, 40%). MS (EI): 186 (MH+).

후처리

  1. stirringshaken
  2. filtrationThe resulting solid was filtered off
  3. washwashed with water
  4. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-d0e0bd4bbee149338404daac09d120bf
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088767B2

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