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

HRID 1051469노트

반응식

HRID 1051469 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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]+

후처리

  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

출처 및 근거

ORD 기록
ord-70bffae8f78a4835a31b4a8750769e7a
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388173B2

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