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Potassium Iodide → 3,4-Bis-octadec-9-enyloxy-benzaldehyde

HRID 604758
ノート
印刷プレビュー

反応式

HRID 604758 の反応式
[CH2:1](Br)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]/[CH:9]=[CH:10]\[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18].[C:20](=[O:23])([O-])[O-].[K+].[K+].[I-].[K+].[CH3:28][OH:29].C(Cl)(Cl)Cl.[C:34]1(=[O:40])[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1>[Al]>[CH2:1]([O:40][C:34]1[CH:39]=[C:38]([CH:37]=[CH:36][C:35]=1[O:23][CH2:20][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH:8]=[CH:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH:28]=[O:29])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH:9]=[CH:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH3:18]
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

7

反応物 5

HCID 4875Potassium IodideHCID 7967CyclohexanoneHCID 11430Potassium CarbonateHCID 58403839-Octadecene, 1-bromo-, (9Z)-2 回HCID 21584188Chloroform methanol

生成物 1

HCID 862608213,4-Bis-octadec-9-enyloxy-benzaldehyde収率 69%

試薬・触媒・溶媒 1

HCID 5359268Aluminum溶媒

反応条件

温度
100 °C

実験手順

To a solution of oleyl bromide (1.8 g, 5.4 mmol) in cyclohexanone (20 ml) was added protocatachualdehyde (0.341 g, 2.5 mmol), potassium carbonate (1.02 g, 7.4 mmol) and potassium iodide (0.05 g, 0.3 mmol). The suspension was stirred at 100° C. for 18 hours under nitrogen. Due to the light sensitivity of the oleyl bromide the flask was covered in aluminum foil. TLC (10% MeOH/CHCl3) showed the reaction was complete. The hot reaction mixture was filtered to remove some of the particulates and the solvent was removed in vacuo. The residue was dissolved in CHCl3 (100 mL) and washed with water (2×75 mL). The CHCl3 layer was dried over anhydrous sodium sulphate, filtered and the solvent removed in vacuo to give a dark yellow oil. The oily residue was purified by flash column chromatography (5% EtAc/hexane) to yield the product 8a as a white solid (1.08 g, 69%), Rf=0.3 (5% EtAc/hexane). 1H NMR (CDCl3) d 9.80 (s, 1H, CHO), 7.37 (m, 2H, phenyl), 6.93 (d, 1H, phenyl), 5.33 (t, 4H, olefinic), 4.06 (t, 2H, OCH2), 4.04 (t, 2H, OCH2), 2.01 (m, 8H, CH2C═C), 1.85 (m, 4H, CH2CH2O), 1.50-1.18 (m, 44H, 22×CH2), 0.88 (t, 6H, CH3); 13C NMR (CDCl3) d 191.00, 155.34, 149.95, 130.14, 130.12, 129.97, 126.79, 111.89, 111.04, 69.36, 32.29, 30.16, 29.92, 29.90, 29.88, 29.72, 29.64, 29.62, 29.44, 29.36, 27.60, 26.37, 26.34, 23.09, 14.53; HRMS (FAB): theory for C43H75O3 (M+1), 639.5716; found (M+1), 639.5755. Anal. (C43H74O3): C, H.

後処理

  1. filtrationThe hot reaction mixture was filtered
  2. customto remove some of the particulates
  3. customthe solvent was removed in vacuo
  4. dissolutionThe residue was dissolved in CHCl3 (100 mL)
  5. washwashed with water (2×75 mL)
  6. dry with materialThe CHCl3 layer was dried over anhydrous sodium sulphate
  7. filtrationfiltered
  8. customthe solvent removed in vacuo
  9. customto give a dark yellow oil
  10. customThe oily residue was purified by flash column chromatography (5% EtAc/hexane)

出典と根拠

ORDレコード
ord-a3f5a0396a1c4aaa85087dc35ae4ddfb
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07910363B1

反応ノート

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