Hydrochloric Acid → 1,5-Bis(4-methoxyphenyl)pentane

HRID 979063ノート

反応式

HRID 979063 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][C:11](=O)[CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[CH:5][CH:4]=1.O1CCOCC1.Cl>[Zn].O>[CH3:21][O:20][C:17]1[CH:16]=[CH:15][C:14]([CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=2)=[CH:19][CH:18]=1

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 312751,4-DioxaneHCID 2801509HCID 2801509、化合物

生成物 1

HCID 132200991,5-Bis(4-methoxyphenyl)pentane収率 111%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 962Water溶媒

実験手順

A mixture of 1,5-bis(4-methoxyphenyl)pentan-3-one of Example 7 (57 g, 0.19 mole), amalgamated zinc (200 g), dioxane (250 ml), concentrated hydrochloric acid (250 ml) and 150 ml of water was refluxed overnight. A further 50 ml of concentrated hydrochloric acid was added after the first 6 hours. The organic layer was separated, diluted with ether, washed with water, dried over anhydrous magnesium sulfate and concentrated to give 60 g of a thick oil. NMR and mass spectra confirmed the structure.

後処理

  1. temperaturewas refluxed overnight
  2. customThe organic layer was separated
  3. additiondiluted with ether
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-664cca7836f34f31996087dc05955dff
出典データセット
uspto-grants-1987_05
特許番号
US04666909

反応ノート

読み込み中…