Methanesulfonic Acid → 2-(5-Bromo-2-chlorophenyl)-1H-benzo[d]imidazole

HRID 77067

반응식

HRID 77067 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:11])=[C:6]([CH:10]=1)[C:7](O)=O.[C:12]1([NH2:19])[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[NH2:18].CS(O)(=O)=O>[OH-].[Na+]>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:11])=[C:6]([C:7]2[NH:19][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[N:18]=2)[CH:10]=1

참가 물질

5

반응물 3

HCID 6395Methanesulfonic AcidHCID 7243O-PhenylenediamineHCID 331275-Bromo-2-chlorobenzoic acid

생성물 1

HCID 433790662-(5-Bromo-2-chlorophenyl)-1H-benzo[d]imidazole

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

반응 조건

온도
170 °C

실험 절차

Method 2—Step a Into a one necked round bottomed flask equipped with a magnetic stirrer, 5-bromo-2-chlorobenzoic acid (70.0 g, 297.3 mmol), o-phenylenediamine (64.3 g, 594.6 mmol) and methansulfonic acid (140 mL) were placed and heated to 170° C. in order to melt the solids. The system was stirred 5 h at this temperature, then left to come rt. The blue solid was treated with NaOH 35% (200 mL) obtaining a violet suspension (pH 5) that was filtered and washed with NaOH 0.5 M (2 L) and H2O (2 L). The product was dried under vacuum (60° C.), to give 61.6 g of a pure violet solid. (67%).

후처리

  1. customMethod 2—Step a Into a one necked round bottomed flask equipped with a magnetic stirrer
  2. waitleft
  3. customto come rt

출처 및 근거

ORD 기록
ord-92bb9cd27d924c84a9817c351b1d9db8
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835648B2

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