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

HRID 1683721노트

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HRID 1683721 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 wo hours until the product which has initially precipitated is completely dissolved. Cool and filter. Concentrate the mother liquors and add petroleum ehter. Combie 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 wo 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 ehter
  10. customCombie 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-771fdf85b83348c9a668a315d8e78fef
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05639756

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