1,1'-Carbonyldiimidazole → 5-Bromo-1,3-dihydro-2H-benzimidazol-2-one

HRID 1051469ノート

反応式

HRID 1051469 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([NH2:9])[C:5]([NH2:8])=[CH:6][CH:7]=1.C1N=CN([C:15](N2C=NC=C2)=[O:16])C=1>O1CCOCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]2[NH:8][C:15](=[O:16])[NH:9][C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 3235934-Bromobenzene-1,2-diamine

生成物 1

HCID 122280605-Bromo-1,3-dihydro-2H-benzimidazol-2-one収率 128%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

The mixture of 4-bromobenzene-1,2-diamine (200 mg, 1.1 mmol), CDI (174 mg, 1.1 mmol) in dioxane was reacted at 50° C. for 16 hours. The mixture was concentrated and the residue was dissolved in DCM and extracted with water with the combined organic phases dried by Na2SO4 and concentrated to give 300 mg of crude product which was used without further purification. LCMS (m/z): 213.1/214.1 [M+H]+/[M+2H]+

後処理

  1. customwas reacted at 50° C. for 16 hours
  2. concentrationThe mixture was concentrated
  3. dissolutionthe residue was dissolved in DCM
  4. extractionextracted with water with the combined organic phases
  5. dry with materialdried by Na2SO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-70bffae8f78a4835a31b4a8750769e7a
出典データセット
uspto-grants-2016_07
特許番号
US09388173B2

反応ノート

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