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Potassium Iodide → 1,1'-(Fluoranthene-3,9-diyl)bis[4-(diethylamino)butan-1-one]--hydrogen chloride (1/2)

HRID 268522
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HRID 268522 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:8]=[CH:9][C:10]2[C:11]3[C:16]([C:17]4[C:22]=2[C:21]=1[CH:20]=[CH:19][CH:18]=4)=[CH:15][CH:14]=[C:13]([C:23](=[O:28])[CH2:24][CH2:25][CH2:26]Cl)[CH:12]=3)=[O:6].[CH2:29]([NH:31][CH2:32][CH3:33])[CH3:30].[I-].[K+]>O1CCCC1>[ClH:1].[ClH:1].[CH2:29]([N:31]([CH2:32][CH3:33])[CH2:2][CH2:3][CH2:4][C:5]([C:7]1[CH:8]=[CH:9][C:10]2[C:11]3[C:16]([C:17]4[C:22]=2[C:21]=1[CH:20]=[CH:19][CH:18]=4)=[CH:15][CH:14]=[C:13]([C:23](=[O:28])[CH2:24][CH2:25][CH2:26][N:31]([CH2:32][CH3:33])[CH2:29][CH3:30])[CH:12]=3)=[O:6])[CH3:30]
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참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 8021DiethylamineHCID 515665HCID 515665, 화합물

생성물 1

HCID 681400271,1'-(Fluoranthene-3,9-diyl)bis[4-(diethylamino)butan-1-one]--hydrogen chloride (1/2)

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 15.0 g (0.037 mole) of 3,9-bis(4-chlorobutyryl)fluoranthene, 100 ml of diethylamine, 2.0 g of potassium iodide and 100 ml of tetrahydrofuran (THF) is heated at reflux with stirring for 3 days and filtered. The filtrate is poured onto ice water and the oil which separates is decanted and dissolved in ether. The ether solution is washed with a water-saturated sodium chloride solution, dried over magnesium sulfate and filtered. The filtrate is acidified with ethereal HCl, and the resulting precipitate is recrystallized twice from methanol-butanone to yield 3,9-bis(4-diethylaminobutyryl)fluoranthene dihydrochloride. M.P. 236°-239°C.

후처리

  1. temperatureat reflux
  2. filtrationfiltered
  3. additionThe filtrate is poured onto ice water
  4. customthe oil which separates is decanted
  5. dissolutiondissolved in ether
  6. washThe ether solution is washed with a water-saturated sodium chloride solution
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customthe resulting precipitate is recrystallized twice from methanol-butanone

출처 및 근거

ORD 기록
ord-a4ab6c152c884c3686a65f875dc0fac8
출처 데이터셋
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03947593

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