Hydrogen Bromide → 2-bromo-5,6-dichloro-1H-benzimidazole

HRID 263856

反応式

HRID 263856 の反応式
N[C:2]1[NH:3][C:4]2[CH:10]=[C:9]([Cl:11])[C:8]([Cl:12])=[CH:7][C:5]=2[N:6]=1.[BrH:13].N([O-])=O.[Na+]>O>[Br:13][C:2]1[NH:3][C:4]2[CH:10]=[C:9]([Cl:11])[C:8]([Cl:12])=[CH:7][C:5]=2[N:6]=1

参加物

5

反応物 3

HCID 260Hydrogen BromideHCID 4660162-Amino-5,6-dichlorobenzimidazoleHCID 23668193Sodium Nitrite

生成物 1

HCID 4660172-bromo-5,6-dichloro-1H-benzimidazole収率 26%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-Amino-5,6-dichlorobenzimidazole (3 g, 16 mmole) was suspended in 150 ml of water and brought into solution with 2 ml of HBr. Sodium nitrite (3.3 g, 55 mmole) was then added and the mixture was stirred at room temperature for 1 hr. Excess CuBr2 was then added and the mixture was heated on a steam bath for 1 hr. The aqueous solution was extracted with ethyl acetate (3×100 ml), dried with MgSO4, concentrated, and crystallized from ethyl ether to give 1.13 g (26%) of 2-bromo-5,6-dichlorobenzimidazole (7).

後処理

  1. temperaturethe mixture was heated on a steam bath for 1 hr
  2. extractionThe aqueous solution was extracted with ethyl acetate (3×100 ml)
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated
  5. customcrystallized from ethyl ether

出典と根拠

ORDレコード
ord-9c0336e43b644f479f0e2f1d41d27327
出典データセット
uspto-grants-1997_07
特許番号
US05646125

関連ノート

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