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

HRID 415124

反応式

HRID 415124 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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+).

後処理

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

出典と根拠

ORDレコード
ord-d0e0bd4bbee149338404daac09d120bf
出典データセット
uspto-grants-2012_01
特許番号
US08088767B2

関連ノート

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