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Ammonium Persulfate → HCID 22117145、化合物

HRID 1275539
ノート
印刷プレビュー

反応式

HRID 1275539 の反応式
[C:1]([O:9][C:10]1[C:11](=[O:21])[C:12]2[C:17]([C:18](=[O:20])[CH:19]=1)=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:22][Si:23]([CH:26](C)[C:27](O)=O)([CH3:25])[CH3:24].S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>C(#N)C.O.C(OCC)C.[N+]([O-])([O-])=O.[Ag+]>[C:1]([O:9][C:10]1[C:11](=[O:21])[C:12]2[C:17]([C:18](=[O:20])[C:19]=1[CH2:27][CH2:26][Si:23]([CH3:25])([CH3:24])[CH3:22])=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 62648Ammonium PersulfateHCID 825051HCID 825051、化合物HCID 12218619HCID 12218619、化合物

生成物 1

HCID 22117145HCID 22117145、化合物収率 46.4%

試薬・触媒・溶媒 4

HCID 24470Silver Nitrate触媒HCID 962Water溶媒
HCID 3283
Diethyl Ether
溶媒
HCID 6342Acetonitrile溶媒

反応条件

温度
65 °C

実験手順

2-Benzoyloxy-1,4-naphthoquinone (1.39 g, 5 mmol), trimethylsilylpropionic acid (1.09 g, 7.5 mmol) and silver nitrate (523 mg, 3 mmol) were suspended in 40 ml aqueous acetonitrile (1:1) and then heated to 65° C. Ammonium persulphate (1.71 g, 7.5 mmol) in 20 ml water was added slowly and dropwise over 30 minutes to the mixture. The reaction mixture was stirred at this temperature for a further hour and then cooled, diluted with diethyl ether and the aqueous phase removed. The organic extract was washed with saturated sodium bicarbonate solution, then brine and dried over anhydrous magnesium sulphate. After concentration in vacuo, the crude material was chromatographed using petroleum ether/ethyl acetate as eluent to give 2-benzoyloxy-3-(2'-trimethylsilylethyl)-1,4-naphthoquinone (879 mg) which was recrystallised from methanol, m.pt.: 92-95° C. NMR peaks at: 184.4, 178.2, 150.3, 142.6, 134.0, 133.8, 132.1, 130.9, 126.6, 126.6; 18.8, 16.2; -2.0; 163.8, 128.0, 128.7, 130.4, 134.2 (PhCO).

後処理

  1. temperaturecooled
  2. customthe aqueous phase removed
  3. extractionThe organic extract
  4. washwas washed with saturated sodium bicarbonate solution
  5. dry with materialbrine and dried over anhydrous magnesium sulphate
  6. concentrationAfter concentration in vacuo
  7. customthe crude material was chromatographed

出典と根拠

ORDレコード
ord-e68e4fa1be104e00b5ec9c0d5fb52ed6
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06162799

反応ノート

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