Trichloroacetyl chloride → 2,9-Dimethyl-3-trichloroacetylimidazo[1,2-a]benzimidazole

HRID 54699노트

반응식

HRID 54699 반응식
[Cl:1][C:2]([Cl:7])([Cl:6])[C:3](Cl)=[O:4].[CH3:8][C:9]1[N:10]=[C:11]2[N:15]([CH:16]=1)[C:14]1[CH:17]=[CH:18][CH:19]=[CH:20][C:13]=1[N:12]2[CH3:21]>C1(C)C(C)=CC=CC=1>[CH3:8][C:9]1[N:10]=[C:11]2[N:15]([C:16]=1[C:3](=[O:4])[C:2]([Cl:7])([Cl:6])[Cl:1])[C:14]1[CH:17]=[CH:18][CH:19]=[CH:20][C:13]=1[N:12]2[CH3:21]

참가 물질

4

반응물 2

HCID 6420Trichloroacetyl chlorideHCID 8282692,4-Dimethylimidazo[1,2-a]benzimidazole

생성물 1

HCID 190408122,9-Dimethyl-3-trichloroacetylimidazo[1,2-a]benzimidazole

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

Pour 5.45 g (30 mmol) of freshly distilled trichloroacetyl chloride dropwise into a boiling solution of 2,9-dimethylimidazo[1,2-a]benzimidazole (3.7 g; 20 mmol)--obtained as described in Khim. Geterotsikl Soedin, 86, (7), 918-925--in 50 ml of xylene, with vigorous stirring, over a period of 20 to 30 minutes. The mixture is then heated at reflux for two hours until the product which has initially precipitated is completely dissolved. Cool and filter. Concentrate the mother liquors and add petroleum ether. Combine with the precipitate obtained earlier and repeat the operation. The combined precipitates are treated with an aqueous solution of sodium hydrogen carbonate and then recrystallised from ethyl acetate.

후처리

  1. customobtained
  2. temperatureThe mixture is then heated
  3. temperatureat reflux for two hours until the product which
  4. customhas initially precipitated
  5. dissolutionis completely dissolved
  6. temperatureCool
  7. filtrationfilter
  8. concentrationConcentrate the mother liquors
  9. additionadd petroleum ether
  10. customCombine with the precipitate obtained earlier
  11. customThe combined precipitates
  12. additionare treated with an aqueous solution of sodium hydrogen carbonate
  13. customrecrystallised from ethyl acetate

출처 및 근거

ORD 기록
ord-61de2979af5447788006ba4dcceb3672
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05623073

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