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Sodium Sulfite → Sodium 7-(2,4,5-tri-phenylimidazol-1-yl)heptane-sulphonate

HRID 265394
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HRID 265394 반응식
[C:1]1([C:7]2[N:8]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30]Br)[C:9]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[N:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[S:32]([O-:35])([O-:34])=[O:33].[Na+:36].[Na+]>C(O)C.O>[C:1]1([C:7]2[N:8]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][S:32]([O-:35])(=[O:34])=[O:33])[C:9]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[N:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Na+:36]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24437Sodium SulfiteHCID 229163771-(7-Bromoheptyl)-2,4,5-triphenylimidazole

생성물 1

HCID 23679429Sodium 7-(2,4,5-tri-phenylimidazol-1-yl)heptane-sulphonate수율 32.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

2,4,5-Triphenyl-1-(7-bromoheptyl)imidazole (0.95 g) was dissolved in hot ethanol (10 ml) and a solution of sodium sulphite (0.38 g) in hot water (5 ml) was added. The white suspension was heated at reflux temperature for 20 hours then evaporated to dryness. The mixture was taken up in dichloromethane, filtered and the filtrate evaporated to an oil which was chromatographed on silica gel (dichloromethane/methanol). The resulting oil was dissolved in methanol and excess ether added giving an oil which slowly solidified to give sodium 7-(2,4,5-tri-phenylimidazol-1-yl)heptane-sulphonate (0.32 g; 32%) as a white solid, m.p. 310° C.

후처리

  1. temperatureThe white suspension was heated
  2. temperatureat reflux temperature for 20 hours
  3. customthen evaporated to dryness
  4. filtrationfiltered
  5. customthe filtrate evaporated to an oil which
  6. customwas chromatographed on silica gel (dichloromethane/methanol)
  7. dissolutionThe resulting oil was dissolved in methanol
  8. additionexcess ether added
  9. customgiving an oil which

출처 및 근거

ORD 기록
ord-34cd3fdd468a46808ed1ed3e5507a979
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05648373

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