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1,3-Dibromopropane → 3-(3-Bromopropyl)-5-(3,5-di-tert-butyl-4-hydroxyphenyl)-1,3,4-oxadiazol-2(3H)-one

HRID 609891
ノート
印刷プレビュー

反応式

HRID 609891 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([C:16]2[O:20][C:19](=[O:21])[NH:18][N:17]=2)[CH:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[OH:11])([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[Na+].[Na+].[Br:28][CH2:29][CH2:30][CH2:31]Br>CN(C)C=O>[Br:28][CH2:29][CH2:30][CH2:31][N:18]1[N:17]=[C:16]([C:7]2[CH:8]=[C:9]([C:12]([CH3:14])([CH3:15])[CH3:13])[C:10]([OH:11])=[C:5]([C:1]([CH3:2])([CH3:3])[CH3:4])[CH:6]=2)[O:20][C:19]1=[O:21]
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 3

HCID 80011,3-DibromopropaneHCID 10340Sodium CarbonateHCID 1355035925-(3,5-di-tert-butyl-4-hydroxyphenyl)-1,3,4-oxadiazol-2(3H)-one

生成物 1

HCID 1357527423-(3-Bromopropyl)-5-(3,5-di-tert-butyl-4-hydroxyphenyl)-1,3,4-oxadiazol-2(3H)-one収率 63.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 5-(3,5-di-tert-butyl-4-hydroxyphenyl)-1,3,4-oxadiazol-2(3H)-one (0.50 g) in dimethylformamide (8 ml) were added sodium carbonate (0.36 g) and 1,3-dibromo-propane (1.74 g), followed by stirring at room temperature for 5 hours. After completion of the reaction, the reaction mixture was poured into ice-water, and the product was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent; chloroform) and then recrystallized from chloroform/n-hexane to afford 0.45 g (63%) of the title compound as colorless crystals. mp 130-131° C. NMR (CDCl3) (200 MHz) δ: 1.46 (18H, s), 2.1-2.6 (2H, m), 3.46 (2H, t, J=6.6 Hz), 3.93 (2H, t,J=6.6 Hz), 5.60 (1H, s), 7.63 (2H, s)

後処理

  1. customAfter completion of the reaction
  2. extractionthe product was extracted with ethyl acetate
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (eluent; chloroform)
  6. customrecrystallized from chloroform/n-hexane

出典と根拠

ORDレコード
ord-c6ceab8309fc421aa2d20459064a55df
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998452

反応ノート

読み込み中…

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