Tetrafluoroborate → 4-(3-Fluoro-6-phenylimidazo[1,2-a]pyrimidin-7-yl)benzaldehyde

HRID 503731

반응식

HRID 503731 반응식
[C:1]1([C:7]2[C:8]([C:16]3[CH:23]=[CH:22][C:19]([CH:20]=[O:21])=[CH:18][CH:17]=3)=[N:9][C:10]3[N:11]([CH:13]=[CH:14][N:15]=3)[CH:12]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.ClC[N+]12CC[N+]([F:34])(CC1)CC2.F[B-](F)(F)F>C(Cl)(Cl)Cl.O.ClCCl>[F:34][C:13]1[N:11]2[CH:12]=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[C:8]([C:16]3[CH:17]=[CH:18][C:19]([CH:20]=[O:21])=[CH:22][CH:23]=3)=[N:9][C:10]2=[N:15][CH:14]=1

참가 물질

7

반응물 3

HCID 26255Tetrafluoroborate2회HCID 27249341-(Chloromethyl)-4-fluoro-1,4-diazoniabicyclo(2.2.2)octane2회HCID 866306554-(6-Phenylimidazo[1,2-a]pyrimidin-7-yl)benzaldehyde

생성물 1

HCID 866306594-(3-Fluoro-6-phenylimidazo[1,2-a]pyrimidin-7-yl)benzaldehyde

시약·촉매·용매 3

HCID 962Water용매HCID 6212Chloroform용매HCID 6344Dichloromethane용매

반응 조건

온도
120 °C

실험 절차

500 mg 4-(6-phenylimidazo[1,2-a]pyrimidin-7-yl)benzaldehyde (prepared as described under example 1) and 880 mg 1-chloromethyl-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate are dissolved in 25 ml chloroform and heated under microwave irradiation to 120° C. After for 45 min and 4 h additional portions of 200 mg of 1-chloromethyl-4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate are added and heating continued at 120° C. The reaction is worked up after 5 h by diluting with water and extraction with dichloromethane. The combined organic layers are dried over Na2SO4 and the solvens evaporated. The crude material is purified on silica gel (dichloromethane/ethyl acetate.

후처리

  1. temperatureheating
  2. customcontinued at 120° C
  3. waitThe reaction is worked up after 5 h
  4. dry with materialThe combined organic layers are dried over Na2SO4
  5. customthe solvens evaporated
  6. customThe crude material is purified on silica gel (dichloromethane/ethyl acetate

출처 및 근거

ORD 기록
ord-1ffb796b817d4d5aaf541cc1292ec535
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776864B2

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