p-Anisoyl chloride → (2-Butyl-5-nitrobenzofuran-3-yl)(4-methoxyphenyl)methanone

HRID 1588743

반응식

HRID 1588743 반응식
[Sn](Cl)(Cl)(Cl)Cl.[CH2:6]([C:10]1[O:11][C:12]2[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][C:13]=2[CH:14]=1)[CH2:7][CH2:8][CH3:9].[C:22](Cl)(=[O:31])[C:23]1[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][CH:24]=1>ClC(Cl)C>[CH2:6]([C:10]1[O:11][C:12]2[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][C:13]=2[C:14]=1[C:22](=[O:31])[C:23]1[CH:28]=[CH:27][C:26]([O:29][CH3:30])=[CH:25][CH:24]=1)[CH2:7][CH2:8][CH3:9]

참가 물질

5

반응물 3

HCID 7477p-Anisoyl chlorideHCID 24287Tin tetrachlorideHCID 98373582-Butyl-5-nitrobenzofuran

생성물 1

HCID 22595055(2-Butyl-5-nitrobenzofuran-3-yl)(4-methoxyphenyl)methanone

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

반응 조건

온도
23 °C

실험 절차

59.8 ml (0.50 mole) of tin tetrachloride are added gradually to a solution of 44.5 g (0.2 mole) of 2-n-butyl 5-nitro benzofuran and 44.3 g (0.26 mole) of anisoyl chloride in 308 ml of dichloroethane. The temperature is maintained at 23° C. and stirring is continued for 24 hours. The mixture is poured onto 770 ml of ice-water and extracted 3 times with 150 ml of dichloroethane. The solution is washed with water, 5% sodium hydrogen carbonate solution and again with water. It is evaporated to dryness and the product thus obtained crystallizes rapidly [purity on high performance liquid chromatography (HPLC): 91.69%]. It is recrystallized from 250 ml of isopropanol and 59 g of 2-n-butyl 3-(4-methoxy benzoyl) 5-nitro benzofuran are thus obtained.

후처리

  1. extractionextracted 3 times with 150 ml of dichloroethane
  2. washThe solution is washed with water, 5% sodium hydrogen carbonate solution and again with water
  3. customIt is evaporated to dryness
  4. customthe product thus obtained
  5. customcrystallizes rapidly [purity on high performance liquid chromatography (HPLC): 91.69%]
  6. customIt is recrystallized from 250 ml of isopropanol and 59 g of 2-n-butyl 3-(4-methoxy benzoyl) 5-nitro benzofuran
  7. customare thus obtained

출처 및 근거

ORD 기록
ord-c3e6ac5c3e5e48cebf32b616fa272e08
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05223510

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