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Hydroquinone → Phenol, 2-ethoxy-4-(methoxymethyl)-

HRID 542392
ノート
印刷プレビュー

反応式

HRID 542392 の反応式
C([CH:3](O)[C:4]1[CH:12]=[CH:11][C:9]([OH:10])=[C:6]([O:7][CH3:8])[CH:5]=1)C.S([O-])(O)(=O)=O.[Na+].[C:20]1(C=CC(O)=CC=1)O.C(=O)([O-])O.[Na+].[CH3:33][OH:34]>>[CH3:33][O:34][CH2:3][C:4]1[CH:12]=[CH:11][C:9]([OH:10])=[C:6]([O:7][CH2:8][CH3:20])[CH:5]=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

6

反応物 5

HCID 785HydroquinoneHCID 887MethanolHCID 516892Sodium BicarbonateHCID 516919Sodium BisulfateHCID 3732967HCID 3732967、化合物

生成物 1

HCID 6453284Phenol, 2-ethoxy-4-(methoxymethyl)-収率 56.3%

反応条件

温度
50 °C

実験手順

100 g of ethylvanillyl alcohol (4-hydroxy-3-ethoxybenzyl alcohol) are dissolved in 200 ml of methanol. The solution is treated with 10 g of sodium hydrogen sulphate and a knife tip of hydroquinone. The mixture is firstly heated to 50° C. for 2 minutes and left to cool again to room temperature. The methanolic solution is now poured into 85 ml of a saturated sodium hydrogen carbonate solution. The methyl alcohol is distilled off in vacuo, the residue is taken up in toluene, the organic solution is washed neutral with water and evaporated. The residue (95.5 g) is fractionally distilled. There are obtained 61.1 g of chemically and olfactorily pure 4-hydroxy-3-ethoxybenzyl methyl ether; b.p.=77° C./0.03 mmHg; d420 =1.1084; nD20 =1.529.

後処理

  1. waitleft
  2. temperatureto cool again to room temperature
  3. distillationThe methyl alcohol is distilled off in vacuo
  4. washthe organic solution is washed neutral with water
  5. customevaporated
  6. distillationThe residue (95.5 g) is fractionally distilled

出典と根拠

ORDレコード
ord-437c75b7674c40bbb271caf90f3d3e76
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04657700

反応ノート

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