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

HRID 265394
ノート
印刷プレビュー

反応式

HRID 265394 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-34cd3fdd468a46808ed1ed3e5507a979
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05648373

反応ノート

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